Characterization of vapor-deposited l-leucine nanofilm

X-ray reflective measurements (XRR), atomic force microscopy and single wavelength ellipsometry were used to investigate the optical properties of thin l-leucine films deposited onto silicon substrates. The ellipsometry data (Ψ,Δ) were fitted with a four-layer-model, and the optical refractive index of the l-leucine film measured with ellipsometry was determined to be 1.37. With the conventional effective medium approximation theory and the ellipsometry results, the density of the l-leucine nanofilm was determined to be 70% (0.81 g/cm³) of crystalline l-leucine. This value was in good agreement with the density of 69% (0.80 g/cm³) obtained with XRR measurement. The ellipsometry measurements also enabled us to estimate the surface roughness or absorption layer of the film. This procedure of combined XRR and ellipsometry measurements could be a powerful tool for the determination of the (otherwise hard-to-determine) refractive index in thin organic material films with a rough surface layer.     

Growth and characterization of a new NLO material: l-Glutamic acid hydro bromide [l-GluHBr]

l-(+)-Glutamic acid hydro bromide, an isomorphic salt of l-glutamic acid hydrochloride, was synthesized and the synthesis was confirmed using Fourier transform infrared analysis. Solubility of the material in water was determined. l-Glutamic acid hydro bromide crystals were grown by low temperature solution growth using the solvent evaporation technique. Single crystal X-ray diffraction studies were carried out and the cell parameters, atomic co-ordinates, bond lengths and bond angles were reported. High-resolution X-ray diffraction studies were carried out and good crystallinity for the grown crystal was observed from the diffraction curve. The grown crystals were subjected to dielectric studies. Ultraviolet-visible-near infrared spectral analysis shows good optical transmission in the visible and infrared region of the grown crystals. The second harmonic generation efficiency of l-glutamic acid hydro bromide crystal was determined using the Kurtz powder test and it was found that it had efficiency comparable with that of the potassium di-hydrogen phosphate crystal.     

l-lysine monohydrochloride dihydrate as novel elasto- and electrooptical materials

We have studied optical parametrical effects (electrooptical and elastooptical ones) at wavelength 1150 nm generated by continuous He-Ne laser. We have found that the maximal value of the effective electrooptics coefficient is equal to about 12.6 pm/V and of the elastooptical coefficient was 12 · 10¹⁴ m²/N and was achieved at temperature about 300 K. l-lysine monohydrochloride dihydrate (C₆H₁₄N₂O₂, HCl·2H₂O, LLMHCl), a semiorganic potential nonlinear optically active crystal belongs to noncentrosymmetry class P2₁. FTIR and FT Raman of this crystal have been studied at room temperature. The vibrational spectral characterization has been carried out for different Raman configurations and has been interpreted following existed crystal structural data and factor group analysis. Following the performed analysis it was discovered that the principal role in the observed electrooptics group plays the vibrational bands originating of the functional groups such as [NH₃]⁺, C=O, O-H, C-H, C-N, O-C=O, C-N-C-C ring, C-OH. For elastooptical effects the principal role belongs to the modes situated at 3500-1500 cm^− 1 originating from stretching vibrations of [NH₃]⁺, CH₂, C=O, COO⁻ and C-N groups.     

Crystallization and characterization of nonlinear optical material l-arginine formomaleate

The influence of mixed acids in the growth and characteristic properties of a new nonlinear optical material l-arginine formomaleate abbreviated as LAFM was examined. Single crystal X-ray diffraction analysis was used to calculate the lattice parameters of the crystals. Fourier transform infrared (FTIR) spectroscopy and thermal analysis (DTA, TGA) were performed to study the molecular vibrations and thermal behaviour of the crystals. UV-VIS spectral study shows that LAFM is transparent down to 315 nm and its second harmonic generation efficiency is 1.2 times that of KDP.     

Theoretical investigations of optical properties of l-arginine trifluoroacetate crystal

In order to determine the molecular dipole moment (μ), polarizability (α), and first hyperpolarizability (β) of l-arginine trifluoroacetate (LATF) crystals, a series of basis sets including polarized and diffuse functions have been employed at the framework of Hartree–Fock and second order Möller–Plesset perturbation theory methods. The MP2/6-311++G(d,p) model predicts for the converged value of in-crystal dipole moment, polarizability and first hyperpolarizability are 21.2 D, 20.0 × 10⁻²⁴ esu and 50.0 × 10⁻³¹ esu, respectively. The calculated HOMO and LUMO energies show that charge transfer occur within the molecule. Electronic excitation properties are discussed within the framework of the two-level model on the basis of an orbital analysis. The coupled perturbed Hartree–Fock (CPHF) procedure yields information on the dispersion behavior of first hyperpolarizability terms. The magnitudes of the various hyperpolarizability terms which describe the various second-order nonlinear processes show the following trend: β(−2ω;ω,ω) > β(0;ω,−ω) > β(0,0,0). By using the molecular structures and the molecular first hyperpolarizability, the components of second harmonic tensor coefficient d of the crystals were evaluated by the oriented-gas model.     

Growth and characterization of l-proline cadmium chloride monohydrate single crystals

A novel semi-organic material of l-proline cadmium chloride monohydrate (l-PCCM) has been successfully synthesized and single crystal was grown by slow evaporation solution growth technique at room temperature. The grown single crystals have been characterized by different instrumentation techniques like XRD, FTIR, UV-Vis-NIR and TG/DTA measurements. Its nonlinear optical property has been tested by Kurtz powder method. The mechanical properties of grown crystals have been studied using Vickers microhardness tester. Its relative SHG efficiency is two times higher than that of potassium dihydrogen phosphate (KDP) single crystal.     

In vitro hydrolytic degradation of poly(para-dioxanone)/poly(d,l-lactide) blends

A series of biodegradable polymers were prepared by solution coprecipitation of poly(para-dioxanone) (PPDO) and poly(d,l-lactide) (PDLLA) in various blend ratios. Samples were compression molded into bars using a platen vulcanizing press. The in vitro hydrolytic degradation of PPDO/PDLLA blends was studied by examining the changes in weight, water absorption, tensile strength, breaking elongation, thermal properties, and morphology of the blends in phosphate buffered saline (PBS; pH 7.44) at 37 °C for 8 weeks. During the hydrolytic degradation, the weight loss and water absorption increased significantly for all samples, whereas the hydrolysis rate varied with the blend composition. The weight loss of PPDO/PDLLA 80/20, which showed the smallest degradation rate, was lower than that of pure PPDO for almost all of the hydrolytic degradation period. The results showed that the blend composition played an important role in determining the degradation behaviors of blends.     

Interfacial bonding of Flax fibre/Poly(l-lactide) bio-composites

The use of glass fibre reinforced polyester composites raises many health and safety and environmental questions. One alternative is the development of high performance bio-based bio-composites with low environmental impact. Improved understanding of interfacial properties is essential to optimise the mechanical properties and durability of these materials, but so far few data are available. The present work describes the interfacial characterization of Flax fibre/Poly(lactic) acid (PLLA) system at the micro-scale using the microbond test. Different thermal treatments have been carried out (cooling rate and annealing) in order to evaluate the influence of matrix and interfacial morphologies as well as residual stress on interfacial properties. Micromechanical models have been used to determine the interfacial shear strength. When cooling rate is slow, improved interfacial properties are observed.     

Facile and controllable one-step fabrication of selenium nanoparticles assisted by l-cysteine

A simple and solution-phase approach for large-scale synthesis of selenium nanoparticles (Nano-Se) by reducing sodium selenite (Na₂SeO₃) with l-cysteine has been demonstrated in this study. l-cysteine was used as both the reducing agent and surface modifier to control the formation of Nano-Se. The effects of reactant concentrations and ratios, and reaction time on the size and stability of Nano-Se were also investigated. The morphology and chemical composition of Nano-Se were characterized using various spectroscopic and microscopic methods. The results showed that varying the concentration ratio of l-cysteine to Na₂SeO₃ could control the diameter and morphology of Nano-Se, but not affecting their crystalline phases and chemical compositions. Monodisperse and homogeneous spherical Nano-Se with an average diameter of about 100 nm could be synthesized with the concentration ratio of l-cysteine to Na₂SeO₃ at 4:1. A striking feature of the as-synthesized Nano-Se was their good stability when dispersed in the reaction solutions, which indicates their potential in medical applications.     

Preparation of poly (l-lactic acid) microspheres by droplet-freezing process

A recently developed process of microsphere preparation, named droplet-freezing process is introduced in this paper. The PLLA microspheres were fabricated by the droplet-freezing process, the diameter and porosity of the microspheres were measured, and the micro-morphologies of the microspheres were characterized by scanning electron microscopy (SEM). The formation process of microspheres was achieved by two steps: first, after droplets dropped off the delivery tube, they became approximately spherical in the air under the effect of the surface tension; second, droplets dropped into liquid condensate and maintained the spherical shape, and were frozen during the free settling process. Experimental results indicated that the microspheres fabricated by the droplet-freezing process have uniform diameters and the diameter can be controlled properly, along with the increase of the PLLA concentration, the size of microspheres increases, but the porosity of the microspheres decreases. The microspheres with high porosity can be obtained with a low concentration of the PLLA solution. SEM analysis revealed that the surfaces and interiors of the microsphere contain plentiful and interconnected micro pores. The microspheres are hopeful to be applied in bone tissue engineering.     

L-Aspartic acid/L-cysteine/gold nanoparticle modified microelectrode for simultaneous detection of copper and lead

This paper presents an electrochemical microsensor for simultaneous detection of copper (II) and lead (II) using an l-aspartic acid/l-cysteine/gold nanoparticle modified microelectrode. The microelectrode was fabricated by Micro Electro-Mechanical System technique. The complex of gold nanoparticles (AuNPs) and amino acid with carboxyl group was used as the selective ligand for metal ions. The microelectrode was firstly modified with AuNPs to increase the sensitive area of the working electrode. Subsequently, the AuNPs/gold electrode was modified with l-cysteine and then covalently linked with a monolayer of l-aspartic acid using glutaraldehyde. Electrochemical analysis of metal ions was achieved by using square wave voltammetry without stirring. The microsensor exhibited an excellent linear range from 5 μg L^− 1 to 2000 μg L^− 1 with the limit of detection of 1 μg L^− 1. This metal ion detection method based on l-aspartic acid/l-cysteine/gold nanoparticle modified microelectrode is simple, sensitive and it could be used for electrochemical analysis of copper (II) and lead (II).     

Growth and characterization of the nonlinear optical single crystal: l-Lysinium trifluoroacetate

A novel organic nonlinear optical (NLO) crystal, l-lysinium trifluoroacetate (with the molecular formula as (H₃N)⁺CH₂CH₂CH₂CH₂CH(H₃N)⁺COO⁻CF₃COO⁻), was grown by the controlled evaporation of its aqueous solution. The X-ray powder diffraction was used to determine its cell parameters. The calculated results based on the diffraction data reveal that l-lysinium trifluoroacetate belongs to the monoclinic crystallographic system, space group P2₁, with cell parameters: a = 5.698(5), b = 23.542(8), c = 8.500(6) Å, β = 91.62(9)°, V = 1139.96 Å³. The grown crystals were characterized by the elemental analyses, Fourier transform infrared and Raman spectra. Experiments of thermogravimetric (TG) and differential thermal analysis (DTA) were carried out to study its thermal properties. The optical behaviours, including transmission spectrum and second harmonic generation (SHG), were investigated to study its linear and nonlinear optical properties. Optical nonlinearities were analyzed and discussed involved with its crystal structure.     

Concentration dependence of solution crystallization for poly(l-lactide) in p-xylene

The macromolecular chain conformation in solution changes with the solvent and temperature, which will affect the formation of crystalline structure in the subsequent crystallization process. The crystallization behavior of poly(l-lactide) samples prepared from solutions with various concentrations was studied by differential scanning calorimetric and X-ray diffraction. It is found that the sample recovered from a dilute solution exhibits higher crystallinity, higher non-isothermal crystallization temperature and faster crystallization rate. The condensation process of polymer chain in dilute solutions has an influence on the crystallization of polymer in the solid state. This results in the acceleration of the melt crystallization rate and the rise of non-isothermal crystallization temperature of PLLA recovered from the dilute solution.     

Crystal growth and characterization of new nonlinear optical single crystals of l-alaninium fumarate

Amino acid based crystals exhibit excellent nonlinear and electro optical properties. A new nonlinear optical single crystal l-alaninium fumarate (LAF) belonging to the amino acid group was grown by slow evaporation solution growth technique. Single crystal X-ray diffraction study showed that LAF belongs to orthorhombic crystal system. The UV-Vis-NIR spectrum of LAF showed very good transparency in the region from 300 nm to 1100 nm. Fourier transform infrared is used to confirm the presence of various functional groups in the grown crystal. Thermal properties of the LAF crystal were carried out by thermogravimetric analysis (TGA) and differential thermal analysis (DTA) techniques, which indicate that the material does not decompose before melting. The melting point of grown crystal was observed as 267.5 °C by melting point apparatus. The existence of nonlinear optical (NLO) property of LAF was confirmed by second harmonic generation test using Nd:YAG laser fundamental wavelength of 1064 nm.     

Cyclic microwave-assisted synthesis of Cu3BiS3 dendrites using l-cysteine as a sulfur source and complexing agent

Nanostructured Cu₃BiS₃ dendrites were successfully synthesized from CuCl, BiCl₃ and l-cysteine in ethylene glycol (EG), using cyclic microwave radiation (CMR). The phase was detected by X-ray diffraction (XRD) and selected area electron diffraction (SAED), and was in accordance with that obtained by the simulation. Scanning and transmission electron microscopic (SEM and TEM) techniques revealed the gradual transformation of nanoparticles to nanostructured dendrites, due to the increase of microwave power. Photoluminescence of Cu₃BiS₃ dendrites was a blue emission centered at 367 nm.     

Synthesis, growth, and characterization of nonlinear optical material l-arginine iodate crystal

Single crystals of nonlinear optical l-arginine iodate (l-Arg·2HIO₃) (C₆H₁₄N₄O₂·2HIO₃), were successfully grown for the first time by the temperature-lowering method and also by the slow evaporation method at a constant temperature (30 °C) from its aqueous solution at pH value of 6. Crystals were of average dimensions 3 × 2.5 × 1.0 cm³ by optimizing the growth parameters. Initially, solubility studies were carried out for four different solvents such as water, water-methanol, water-ethanol, and water-acetone. Among the four solvents, the solubility of l-Arg·2HIO₃ was found to be the highest in water and hence crystallization of l-Arg·2HIO₃ was carried out from aqueous solution. Morphology studies reveal that the crystals grow with reasonable growth rate along the [100], [001], [110¯] and [011] direction. As-grown crystals were characterized by density measurement, X-ray powder diffraction studies, infrared spectrophotometer, UV-Vis spectrometer, laser induced damage threshold studies and nonlinear optical study.     

Synthesis and characterization of biodegradable poly(l-lactide)/layered double hydroxide nanocomposites

This study reports the preparation and physical properties of biodegradable nanocomposites fabricated using poly(l-lactide) (PLLA) and magnesium/aluminum layered double hydroxide (MgAl-LDH). The MgAl-LDH with molar ratio of Mg/Al = 2 were synthesized by the co-precipitation method. In order to improve the chemical compatibility between PLLA and LDH, the surface of LDH was organically-modified by polylactide with carboxyl end group (PLA–COOH) using ion-exchange process. Then, the PLLA/LDH nanocomposites were prepared by solution intercalation of PLLA into the galleries of PLA–COOH modified LDH (P-LDH) in tetrahydrofuran solution. Both X-ray diffraction data and Transmission electron microscopy images of PLLA/P-LDH nanocomposites indicate that the P-LDHs are randomly dispersed and exfoliated into the PLLA matrix. Mechanical properties of the fabricated 1.2 wt.% PLLA/P-LDH nanocomposites show significant enhancements in the storage modulus when compared to that of neat PLLA. Adding more P-LDH into PLLA matrix induced a decrease in the storage modulus of PLLA/P-LDH nanocomposites, probably due to the excessive content of PLA–COOH moleculars with low mechanical properties. The thermal stability and degradation activation energies of the PLLA and PLLA/P-LDH nanocomposites can also be discussed.     

Growth and characterization of a new non-linear optical l-histidinium dihydrogen phosphate single crystal

New non-linear optical single crystal of l-histidinium dihydrogen phosphate was grown by slow evaporation and temperature lowering technique from aqueous solution. Solubility studies have been carried out for three different solvents (water, acetone and ethanol). The grown crystals have been subjected to single crystal X-ray diffraction analysis to identify the cell parameters and morphology. Optical transmission spectra reveal the optical properties of the grown crystals. The NLO property of the crystal has been confirmed by Kurtz SHG test. Comparing the output power it has been confirmed that l-HDP crystals possess higher SHG efficiency than KDP. Thermal studies were carried out to check the thermal stability of the crystals.     

Growth and characterization of an organic nonlinear optical material: l-alanine alaninium nitrate

l-alanine alaninium nitrate (LAAN), an organic nonlinear optical material was grown by slow evaporation technique at room temperature from its aqueous solution at pH value of 2.5. As grown single crystals were characterized for its spectral, thermal, linear and second order nonlinear optical properties. LAAN crystallizes in monoclinic system with space group P₂₁ and cell parameters a = 7.846 Å, b = 5.431 Å, c = 12.806 Å and β = 94.65°. The mode of vibrations of different molecular groups present in LAAN were identified by FTIR studies. The thermal behaviour of the crystals has been investigated using thermogravimetry (TG) and differential thermal analysis (DTA), which indicates that the material does not decompose before melting. Transmittance spectrum reveals that the crystal has a low UV cut-off of 320 nm and has a good transmittance in the entire visible region. NLO property of the crystal was confirmed by Kurtz SHG powder technique.     

Crystallization kinetics and high-resolution X-ray diffraction analysis on nonlinear optical l-threonine single crystals

Crystallization parameters such as critical radius, critical free energy and volume free energy change have been evaluated for l-threonine single crystals using homogeneous nucleation theory. Metastable zone width and induction period measurements have been carried out experimentally. Interfacial energy values for the aqueous solution of l-threonine were also calculated from the solubility data. Optimization of growth parameters has been tried for bulk crystal growth and it has been discussed in detail. The crystalline quality of the bulk samples grown at different pH values have been tested by high-resolution X-ray diffraction analysis.