Good Quality Single Crystals Research Articles

Smart hydrogel crystal gardens

Growing good-quality single crystals of proteins for high-resolution X-ray diffraction relies on the use of a diverse range of materials as nucleating agents. Smart hydrogels, in the form of molecularly imprinted polymers, may provide a general solution.

Growth, optical, mechanical and dielectric studies on NLO active pure and metal ion doped single crystals of bis-thiourea zinc chloride

Good quality single crystals of pure and metal ion (Ni 2+) doped bis-thiourea zinc chloride (BTZC) possessing excellent nonlinear optical properties have been grown from aqueous solution by the slow solvent evaporation technique. The lattice parameters of the grown crystals are determined by single crystal X-ray analysis. The well defined sharp peaks in the powder X-ray diffraction pattern reveals the crystalline perfection and the EDAX spectrum confirms the presence of dopant in the lattice of the parent crystal. The DRS UV–visible spectral study reveals improved transparency for the doped crystal, ascertaining the inclusion of metal ion in the lattice. The optical band gap of the pure and doped crystals was calculated to be 4.8 and 5.2 eV respectively from the UV transmission spectrum. The vickers hardness test brings forth higher hardness value for Ni 2+doped BTZC as compared to pure BTZC crystal. The dielectric measurement exhibits very low dielectric constant and dielectric loss at higher frequencies for both the pure and Ni 2+doped BTZC. The existence of second harmonic generation signals in the crystal also has been confirmed by performing the Kurtz powder test.

Growth and studies of thiourea urea magnesium chloride (TUMC) single crystals

A new semi organic Non-linear optical (NLO) crystal thiourea urea magnesium chloride (TUMC) was grown by slow evaporation technique at room temperature. Good quality single crystals were grown within 20 days. The FTIR spectrum of title compound was recorded and vibrational assignments were made. The recorded UV–vis spectrum shows the optical transmission property of the crystal. The Second harmonic generation (SHG) of TUMC crystal was tested by Kurtz–Perry method using Nd:YAG laser and the result confirms that the grown crystal exhibits NLO property. To analyse the thermal stability of the crystal TG/DTA analysis were made. Detailed structural analysis of the compound is under progress.

Synthesis, growth and optical properties of semi organic non linear optical single crystal: l-Arginine acetate

In the recent past, nonlinear optical materials are getting attention in the field fibre optic communication and optical signal processing. In the present study, the title compound was successfully synthesized by conventional chemical reaction and then the single crystal was grown by slow evaporation solution growth technique. l-Arginine acetate (LAA) is semi organic non linear optical single crystal and crystallizes in noncentrosymmetric space group. The grown good quality single crystals have been analyzed by different characterization analyses such as powder X-ray diffraction, high resolution X-ray diffraction (HRXRD), Raman spectroscopy, photoluminescence, SEM, micro-hardness, thermal and birefringence analyses.

ChemInform Abstract: Synthesis of ThCr2Si2‐Type Arsenides from Bi Flux.

AbstractLaCo2As2 single crystals of good quality are prepared from a 1:2:2 mixture of La, Co, and As in a Bi flux (evacuated quartz tube, 1173 K, 10 d).

Synthesis, growth and characterization of a new derivative 4-ethoxy-N-methyl-4-stilbazolium besylate monohydrate single crystal

A new organic material 4-ethoxy-N-methyl-4-stilbazolium besylate monohydrate, a derivative in the stilbazolium family, known for efficient nonlinear optical materials, has been synthesized for the first time. Employing the slow evaporation technique, optically transparent good quality single crystals of size 15 mm×10 mm×5 mm were grown from methanol. The cell dimensions obtained by single crystal X-ray diffraction studies reveal that the crystal belongs to the monoclinic system. Functional groups of the grown crystal were identified from FTIR and NMR spectral analysis. UV−vis−NIR studies show that the crystal is transparent in the wavelength range 460–1100 nm. The thermal stability of the compound was determined by thermal analyses of the specimen.

Growth, spectral, and thermal characterization of semicarbazone of p-hydroxy acetophenone (SPHA)

A new organic nonlinear optical material semicarbazone of p-hydroxy acetophenone (SPHA) was synthesized. Good quality single crystal of SPHA was successfully grown by slow evaporation method at room temperature. The crystal system was identified and lattice dimensions were measured from the single crystal X-ray diffraction (XRD) analysis. The various planes of reflection were identified from the powder XRD pattern. The presence of functional groups was qualitatively found by Fourier transform infrared (FTIR) spectral analysis. The proton and carbon nuclear magnetic resonance (1HNMR and 13CNMR) spectral studies confirmed the presence of hydrogen and carbon bonded network in the grown crystal. The UV–Visible absorption spectrum was recorded to study the optical transmittance in the range from 200 to 800 nm. The thermal stability of compound was determined by thermogravimetric and differential thermal analysis (TG-DTA) traces. The existence of second harmonic generation (SHG) signal was observed using Nd:YAG laser with fundamental wavelength of 1064 nm.

High-Throughput Study of the Cu(CH3COO)2·H2O−5-Nitroisophthalic Acid−Heterocyclic Ligand System: Synthesis, Structure, Magnetic, and Heterogeneous Catalytic Studies of Three Copper Nitroisophthalates

A high-throughput screening was employed to identify new compounds in Cu(CH3COO)2·H2O−NIPA−heterocyclic ligand systems. Of the compounds identified, three compounds, [Cu3{(NO2)−C6H3−(COO)2}3(C3N6H6)] (I), [Cu2(μ3-OH)(H2O){(NO2)−C6H3−(COO)2}(CN4H)]·(H2O) (II), and [Cu2(μ3-OH)(H2O){(NO2)−C6H3−(COO)2}(CN5H2)]·2(H2O) (III), have been isolated as good quality single crystals by employing conventional hydrothermal methods. Three other compounds, Cu2{(NO2)−C6H3−(COO)2}(CN4H)(H2O) (IIa), Cu2{(NO2)−C6H3−(COO)2}(CN5H2) (IIIa), and Cu2{(NO2)−C6H3−(COO)2}{(CN5H2)2}2H2O (IIIb), were identified by a combination of elemental analysis, thermogravimetric analysis (TGA), and IR spectroscopic studies, although their structures are yet to be determined. The single crystalline compounds were also characterized by elemental analysis, TGA, IR, UV−vis, magnetic, and catalytic studies. The structures of the compounds have paddle wheel (I) and infinite Cu−O(H)−Cu chains (II and III) connected with NIPA and heterocyclic ligands for...

Synthesis, Characterization and Crystal Structure of N,N′-Bis(2,3-Dimethoxybenzylidene)-1,2-Diaminoethane

Synthesis and characterization of single crys- tals of a new organic Schiff-base derivative, N,N 0 -bis(2, 3-dimethoxybenzylidene)-1,2-diaminoethane is reported. Good quality single crystals with size 10 mm 9 1m m9 1 mm were grown by slow evaporation technique from a methanol solution at room temperature. The grown crystals have been characterized by elemental analyses and func- tional groups were identified using FT-IR and 1 H-NMR spectroscopy. Crystal structure of the title compound has been determined by single crystal X-ray diffraction. The title compound has a monoclinic symmetry, space group P21/c, lattice parameters are a = 4.4159(3) A ˚ , b = 14.2333(9) A ˚ , c = 15.0601(10) A ˚ , b = 97.755(5), Z = 2, V = 937.91(11) A ˚ 3 .

Floating-zone growth and characterization of single crystals of cobalt orthosilicate, Co 2SiO 4

Good quality single crystals of high purity cobalt silicate, Co 2SiO 4, were successfully grown by the floating-zone method in air at atmospheric pressure along the three principle orientations. The grown crystals were 30–60 mm in length and 6–10 mm in diameter. Well developed facets were found on all crystals grown. Impurity levels and the degree of a desired excess of silicon in grown crystals were determined by using the ICP-AES technique. In addition, the presence of a small amount of inclusions in the matrix of grown crystals due to a small excess of silica was confirmed by TEM. Dislocation densities were determined upon etching; the observed densities were on the order of 10 5–10 6 cm −2.

Synthesis, growth, crystal structure and characterization of a new organic material: Glycine glutaric acid

Glycine glutaric acid, a new organic compound has been synthesized and good quality single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal XRD. The presence of the functional groups was confirmed by using FT-IR spectroscopy. The optical transparency was studied by using UV–vis spectrophotometer and it was found that the crystal is having high optical transparency. The thermal stability of the crystal was studied by using thermo-gravimetric and differential thermal analyses and found that it is stable up to 150 °C. The room temperature dielectric studies were also carried out over the wide frequency range: 10 mHz to 10 MHz.

Synthesis and growth of materials for solid state lasers: Nd:YLF and Nd:LLW single crystal fibers

Despite new developments for compact laser devices, the neodymium ion (Nd 3+), continues to be the most widely used active laser ion. In this article, the growth of Nd:LiYF 4 (Nd:YLF) and Nd:LiLa(WO 4) 2 (Nd:LLW) single crystal fibers growth is reported considering their use as laser media. Homogeneous and good optical quality single crystals fibers of both materials were obtained. Additionally, structural and optical characterizations were performed on Nd:LLW single fibers. The dependence of the atmosphere on Nd:YLF fibers growth were also studied. Dopant distribution was measured along the fibers. Loss and gain tests were performed on the fluoride single crystal fiber to prove that laser action is achievable.

Studies on the synthesis, growth, crystal structure, and physical properties of a novel nonlinear optical crystal: Glycine 3,5-dihydroxybenzoic acid

A noncentrosymmetric crystal was prepared from glycine and 3,5-Dihydroxybenzoic acid, which was designed for second harmonic genernation. Good quality single crystals of Glycine and 3,5-Dihydroxybenzoic acid (GDHB) were successfully grown by the slow evaporation method with dimensions 18×5×4mm3. The crystal structure of GDHB has been determined, and it belongs to the noncentrosymmetric space group Pca21. The 1H NMR and 13C NMR spectra were recorded to confirm the molecular structure. Density functional theory at the B3LYP/HF6-31G(d,p) level has been used to compute the first order hyperpolarizability of GDHB. Fourier transform infrared (FTIR) spectral study has been performed to identify the functional groups. Thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) were used to study its thermal properties. Powder test with Nd:YAG laser radiation shows a second harmonic generation. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser.

Growth and characterization of a solution grown, new organic crystal: l-histidine-4-nitrophenolate 4-nitrophenol (LHPP)

Bulk single crystals of l-histidine-4-nitrophenolate 4-nitrophenol (LHPP), a new organic material, have been successfully grown for the first time using slow evaporation solution growth technique at room temperature. Good optical quality single crystal of dimension up to 7×3×2 mm 3 has been obtained. The grown crystals have been analyzed with X-ray diffraction, vibrational spectral and thermal measurements. The Kurtz powder technique has been adopted preliminarily to check the optical nonlinearity of the crystal. Its optical behavior has been examined through UV–vis–NIR absorption and PL emission spectra. They signify that the crystal is transparent in the region between 209 and 1200 nm. To study the quality of the crystal SEM images have been recorded.

Crystal growth and comparison of vibrational and thermal properties of semi-organic nonlinear optical materials

Single crystals of urea thiourea mercuric sulphate (UTHS) and urea thiourea mercuric chloride (UTHC), semi-organic nonlinear optical materials, were grown by low-temperature solution growth technique by slow evaporation method using water as the solvent. Good quality single crystals were grown within three weeks. The nonlinear nature of the crystals was confirmed by SHG test. The UV-Vis spectrum showed the transmitting ability of the crystals in the entire visible region. FTIR spectrum was recorded and vibrational assignments were made. The degree of dopant inclusion was ascertained by AAS. The TGA-DTA studies showed the thermal properties of the crystals.

Growth, Spectral, and Thermal Properties of Organic Nonlinear Optical Active Morpholin-4-ium-Hydroxybenzoate Single Crystal

A nonlinear optical morpholin-4-ium-hydroxybenzoate (M4HB) material has been synthesized. Good quality single crystal of M4HB was successfully grown by slow evaporation method with dimensions 16 × 6 × 5 mm3. The unit cell dimensions were determined from single crystal X-ray diffraction (XRD) studies. XRD analysis confirms that the crystal belongs to the monoclinic system with noncentrosymmetric space group cc. The presence of functional groups was estimated qualitatively by Fourier transform infrared analysis (FTIR). Nuclear magnetic resonance (NMR) (1H and 13C) studies confirm the presence of hydrogen and carbon bonded network in the grown crystal. From the mass spectral studies, it is clear that the peak at m/z 224 corresponds to the molecular ion peak [M+] of the compound. The optical cut-off wave length for this crystal was observed at 220 nm. The thermal stability of compound was determined by thermogravimetric and differential thermal analysis (TG-DTA) traces. The existence of second harmonic generation (SHG) signal was observed using Nd:YAG laser with fundamental wavelength of 1064 nm.

Investigations on the physicochemical properties of 2,4-dinitrophenol: Efficient organic nonlinear optical crystal for frequency doubling

Good quality single crystal of 2,4-dinitrophenol is grown by slow evaporation solution growth technique. The cell parameters are determined from the single crystal X-ray analysis. The characteristic frequencies of the various functional groups are identified by investigating FTIR and FT Raman spectra and they are assigned. The result of thermal analysis reveals the decomposition mechanism and the thermal stability of the compound. Optical transparency in the visible region, the lower cut-off wavelength and the band gap energy are estimated from the optical studies. The first order static hyperpolarizability value is calculated and it is 8.4 times greater than that of the urea. The gap between highest occupied molecular orbital and the lowest unoccupied molecular orbital is calculated, which is useful for estimating the efficiency of second harmonic generation. The crystal exhibits high relative conversion efficiency when compared to urea.

Synthesis, spectral and thermal studies of new nonlinear optical crystal: l-valinium fumarate

An organic nonlinear optical material, l-valinium fumarate (abbreviated as LVF) has been successfully synthesized and good quality single crystals have been grown by low temperature solution growth method. The purified form of LVF is achieved by repeated crystallization. The cell parameters of LVF have been determined using single crystal X-ray diffraction technique and the crystal system is found as monoclinic. From the UV–Vis–NIR absorption spectrum, the good transparency is revealed from 300 nm to 1100 nm. The mode of vibration of different molecular groups present in LVF was identified by FT-IR spectral analysis. The thermogravimetric (TGA) and differential thermal analysis (DTA) studies show the thermal behavior and crystal was thermally stable up to 266 °C. Second harmonic generation (SHG) conversion test was made to explore the nonlinear optical behavior of this material using Kurtz and Perry method.

Controlled vinyl‐type polymerization of norbornene with a Nickel(II) diphosphinoamine/methylaluminoxane catalytic system

AbstractA novel nickel‐based complex coordinated with an asymmetric diphosphinoamine ligand was synthesized and fully characterized. Single crystals of good quality were also obtained, and the solid‐state structure of the complex was studied via X‐rays diffraction. The catalytic activity of this Ni(II) complex in the vinyl‐type polymerization of norbornene was studied with methylaluminoxane (MAO) as the cocatalyst/activator. The influence of the reaction time, the equivalents of MAO used, and the concentration of the monomer on: (i) the activity of the catalytic system; (ii) the isolated yield of the polymer; and (iii) the molecular weight and molecular weight distribution of the polymer were investigated. The isolated polynorbornene (PNB) yields are significantly higher compared with those reported for other similar nickel‐based systems. The as‐obtained PNBs are characterized by high molecular weights and relatively narrow and monomodal molecular weight distributions (amongst the narrowest reported in the literature). The linear dependence of the molecular weight of the obtained PNB on the concentration of norbornene points toward a controlled polymerization reaction. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 5241–5250, 2009

Parametrical optical effects in the 1:1 complex of resorcinol and urea—a non linear optical crystal

Good quality single crystals of a complex between urea and resorcinol (UR–C 6H 5O 2 −:(NH 2)CO(NH 3) +) in the ratio (1:1) have been grown by low temperature solution growth technique using acetone and a mixture of acetone and water (1:1). The solubility studies have been carried out in both the solvents at various temperatures. The X-ray diffraction studies show that the complex crystallized in orthorhombic space group P2 12 12 1. The linear electro optical, piezooptical and second harmonic generation measurements were performed. The results obtained in these studies were discussed in detail. The optical transparency window observed in the visible and near IR regions recommends the crystal for nonlinear optical applications. Dependence of the effective second order optical susceptibility on time of simultaneously applied dc-electric field and UV-treatment were performed and discussed.