Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

NASA Technical Reports Server (NTRS)

Chen, Po-Shou; Wilcox, Roy C.

1990-01-01

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Growth and physicochemical properties of second-order nonlinear optical 2-amino-5-chloropyridinium trichloroacetate single crystals

NASA Astrophysics Data System (ADS)

Renugadevi, R.; Kesavasamy, R.

2015-09-01

The growth of organic nonlinear optical (NLO) crystal 2-amino-5-chloropyridinium trichloroacetate (2A5CPTCA) has been synthesized and single crystals have been grown from methanol solvent by slow evaporation technique. The grown crystals were subjected to various characterization analyses in order to find out the suitability for device fabrication. Single crystal X-ray diffraction analysis reveals that 2A5CPTCA crystallizes in monoclinic system with the space group Cc. The grown crystal was further characterized by Fourier transform infrared spectral analysis to find out the functional groups. The nuclear magnetic resonance spectroscopy is a research technique that exploits the magnetic properties of certain atomic nuclei. The optical transparency window in the visible and near-IR (200--1100 nm) regions was found to be good for NLO applications. Thermogravimetric analysis and differential thermal analysis were used to study its thermal properties. The powder second harmonic generation efficiency measurement with Nd:YAG laser (1064 nm) radiation shows that the highest value when compared with the standard potassium dihydrogen phosphate crystal.

Growth and characterization of benzyl 4-hydroxybenzoate single crystal by vertical Bridgman technique for optical applications

NASA Astrophysics Data System (ADS)

Solanki, S. Siva Bala; Rajesh, N. P.; Suthan, T.

2018-07-01

The benzyl 4-hydroxybenzoate single crystal has been grown by vertical Bridgman technique. The grown crystal was confirmed by single crystal X-ray diffraction studies. The presence of functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) spectral studies. The thermal behaviour of the grown crystal was analyzed by thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) studies. Optical behaviour of the grown benzyl 4-hydroxybenzoate crystal was studied by UV-Vis-NIR spectral analysis. Fluorescence spectrum shows near violet light emission. The second harmonic generation behaviour of benzyl 4-hydroxybenzoate was analyzed. The laser damage threshold value of benzyl 4-hydroxybenzoate was measured as 2.16 GW/cm2. The dielectric measurements of benzyl 4-hydroxybenzoate crystal were carried out with different frequencies 1 kHz to 1 MHz versus different temperatures ranging from 313 to 353 K. Photoconductivity study shows that the grown benzyl 4-hydroxybenzoate crystal belongs to negative photoconductivity property. The mechanical strength of the crystal was calculated by Vickers microhardness study.

Growth of propyl-p-hydroxybenzoate single crystals and its characterizations

NASA Astrophysics Data System (ADS)

Karunagaran, N.; Ramasamy, P.

2012-06-01

Single crystals of Propyl-p-hydroxybenzoate (PHB) crystals have been grown by slow evaporation solution technique (SEST) using methanol as a solvent. The PHB single crystal of dimension up to 27×16×8 mm3 has been grown in a period of 18 days at room temperature. The optical transparency of the grown PHB crystal has been measured on (212) plane by UV-Vis-NIR spectrophotometer. The crystal has 60% of transparency in the entire visible region. The thermo gravimetric analysis (TG) and differential thermal analysis (DTA) studies reveal that the crystal is thermally stable up to 99°C. The mechanical strength of the grown PHB crystal is measured using Vickers microhardness tester. The chemical etching studies were carried out on (212) plane using methanol etchant. The laser damage threshold of PHB crystal is 1.3 GW/cm2. The dielectric properties have been investigated. The birefringence value is found to be 0.10148 at the wavelength of 504 nm. The refractive index of grown PHB single crystal is 1.6753.

Growth and characterization of AgGa0.5In0.5Se2 single crystals by modified vertical Bridgman method

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-05-01

AgGa0.5In0.5Se2 single crystal was grown using a double wall quartz ampoule with accelerated crucible rotation technique by modified vertical Bridgman method. The structural perfection was measured using HRXRD. The grown single crystal composition was measured using ICP-OES analysis and compositional uniformities were measured using Raman spectroscopy analysis. Photoconductivity measurements confirm the positive photoconducting nature.

Studies on 2-amino-5-nitropyridinium nitrate (2A5NPN): A semi-organic third order nonlinear optical single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sivasubramani, V.; Pandian, Muthu Senthil, E-mail: senthilpandianm@ssn.edu.in; Ramasamy, P.

2016-05-23

2-amino-5-nitropyridinium nitrate (2A5NPN) is a semi-organic nonlinear optical crystal and optically good quality 2A5NPN single crystals were successfully grown by slow evaporation solution growth technique (SEST) at ambient temperature. The crystallographic structure of the grown crystal was determined by single crystal X-Ray diffraction analysis and it belongs to Monoclinic crystal system with centro symmetric crystalline nature. The crystallinity of the grown crystal was confirmed by powder X-ray diffraction analysis. The other physical properties of grown crystals are also characterized using TG-DTA, UV-Visible NIR, chemical etching, photoconductivity and Z-scan measurements. The Z-scan method reveals that the 2A5NPN crystal possesses multi photonmore » absorption behaviour and the significantly higher third order susceptibility and it is a promising potential NLO material.« less

Effect of Crystal Orientation on Analysis of Single-Crystal, Nickel-Based Turbine Blade Superalloys

NASA Technical Reports Server (NTRS)

Swanson, G. R.; Arakere, N. K.

2000-01-01

High-cycle fatigue-induced failures in turbine and turbopump blades is a pervasive problem. Single-crystal nickel turbine blades are used because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities. Single-crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant and complicating factor. A fatigue failure criterion based on the maximum shear stress amplitude on the 24 octahedral and 6 cube slip systems is presented for single-crystal nickel superalloys (FCC crystal). This criterion greatly reduces the scatter in uniaxial fatigue data for PWA 1493 at 1,200 F in air. Additionally, single-crystal turbine blades used in the Space Shuttle main engine high pressure fuel turbopump/alternate turbopump are modeled using a three-dimensional finite element (FE) model. This model accounts for material orthotrophy and crystal orientation. Fatigue life of the blade tip is computed using FE stress results and the failure criterion that was developed. Stress analysis results in the blade attachment region are also presented. Results demonstrate that control of crystallographic orientation has the potential to significantly increase a component's resistance to fatigue crack growth without adding additional weight or cost.

Translation effects on vertical Bridgman growth and optical, mechanical and surface analysis of 2-phenylphenol single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sadhasivam, S., E-mail: sadha.phy1@gmail.com; Perumal, Rajesh Narayana

2-phenylphenol optical crystals were grown in cone ampoules using vertical Bridgman technique. Single crystal of 2-phenylphenol with 150 mm length has been grown. The inclination on the conical part of the ampoule reduces the growth defects in the 2-phenylphenol single crystal. The lattice parameters and structure studied using single crystal X-ray diffraction method. 2-phenylphenol single crystal belongs to orthorhombic space group Fdd2. The micro translation rate affects crystal growth of 2-phenylphenol crystal was studied. The translation rate dependent defects present in the crystal were investigated by transmittance, indentation and etching characterizations. The dislocation induced indentation crack lengths variations were studied. Etchmore » pits and striations observed for the selective etchants furnish significant information on growth aspects and degree of defect present in the crystal.« less

Synthesis, growth, structural, optical, luminescence, surface and HOMO LUMO analysis of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate organic single crystals grown by a slow evaporation technique

NASA Astrophysics Data System (ADS)

Karthigha, S.; Kalainathan, S.; Maheswara Rao, Kunda Uma; Hamada, Fumio; Yamada, Manabu; Kondo, Yoshihiko

2016-02-01

Single crystals of 2-[2-(4-cholro-phenyl)-vinyl]-1-methylquinolinium naphthalene-2-sulfonate (4CLNS) were grown by a slow evaporation technique. The formation of molecule was confirmed from 1H NMR and FTIR analysis. The confirmation of crystal structure was done by single crystal XRD and atomic packing of grown crystal was identified. The grown single crystal crystallized in triclinic structure with centrosymmetric space group P-1. The crystalline nature of the synthesised material was recorded by powder XRD. The optical absorption properties of the grown crystals were analyzed by UV-vis spectral studies. The thermal behaviour of the title material has been studied by TG/DTA analysis which revealed the stability of the compound till its melting point 276.7 °C. The third order nonlinear optical property of 4CLNS was investigated in detail by Z scan technique and it confirms that the title crystal is suitable for photonic devices and NLO optical applications. Emissions at 519 nm in green region of the EM spectrum were found by photoluminescence studies. The charge transfer occurring within the molecule is explained by the calculated HOMO and LUMO energies.

Growth and characterization of organic NLO material: Clobetasol propionate

NASA Astrophysics Data System (ADS)

Purusothaman, R.; Rajesh, P.; Ramasamy, P.

2015-06-01

Single crystals of clobetasol propionate (CP) have been grown by slow evaporation solution technique using mixed solvent of methanol-acetone. The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm their lattice parameter and space group. The powder X-ray diffraction pattern of the grown CP has been indexed. Thermal analysis was performed to study the thermal stability of the grown crystals. Photoluminescence spectrum shows broad emission peak observed at 421 nm. Nonlinear optical studies were carried out for the grown crystal and second harmonic generation (SHG) efficiency was found in the crystal.

Structural analysis of benzothienobenzothiophene-based soluble organic semiconducting crystals grown by liquid crystal solvent

NASA Astrophysics Data System (ADS)

Shibata, Yosei; Matsuzaki, Tomoya; Ishinabe, Takahiro; Fujikake, Hideo

2018-06-01

In this study, we analyzed organic semiconducting single crystals composed of benzothienobenzothiophene derivatives (2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene, C8-BTBT) grown by nematic-phase liquid crystal (LC) solvent. As a result, we clarified that the crystal b-axis direction of the C8-BTBT single crystals was consistent with the LC alignment direction. By optical evaluation and simulation based on density functional theory, we found that the C8-BTBT single crystals in LC solvent exhibited a novel molecular conformation having alkyl chains oriented toward the b-axis.

Structural, spectral and birefringence studies of semiorganic nonlinear optical single crystal: Calcium5-sulfosalicylate

NASA Astrophysics Data System (ADS)

Shalini, D.; Kalainathan, S.; Ambika, V. Revathi; Hema, N.; Jayalakshmi, D.

2017-11-01

Semi-organic nonlinear optical crystal Calcium5-Sulfosalicylate (CA5SS) was grown by slow evaporation solution growth technique. The cell parameters and molecular structure of the grown crystal were studied by single crystal x-ray diffraction analysis. The presence of various functional groups of the grown crystal was confirmed using Fourier transform infrared (FT-IR), Fourier transform Raman (FT-Raman) analysis. UV-Visible spectrum shows that CA5SS crystals have high transmittance in the range of 330-900 nm. The refractive index, birefringence and transient photoluminescence properties of the grown crystal were analyzed. The frequency doubling of the grown crystal (CA5SS) were studied and compared with that of KDP.

Optical, structural, thermal and dielectric spectroscopy characterizations of seeded melt grown 2-hydroxy biphenyl single crystal.

PubMed

Sadhasivam, S; Rajesh, Narayana Perumal

2014-09-15

Organic single crystal of 2-hydroxy biphenyl (2-HB) was grown by top seeded melt growth method. Scanning electron microscopy studies has been carried out on the surface of the grown crystals to investigate the nature of growth and defects. The crystalline perfection and lattice parameters of 2-HB has been determined by single crystal XRD analysis and it belongs to orthorhombic crystal system with space group Fdd2. The functional groups and molecular associations were confirmed by FT-IR. The optical characteristics such as cut-off and transmittance were carried out using UV-Vis-NIR spectra. Absence of absorption in the region between 320 and 1100 nm makes the grown crystal desirable to optical applications. Thermal stability of grown crystals was characterized by thermogravimetric (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) analyses. Broadband dielectric studies reveals that dielectric constant of grown crystal is low. The resistivity of grown crystal was studied by impedance analysis. The second harmonic generation intensity of 3.8 mJ was studied. The grown crystal belongs to soft material studied by hardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

Growth and characterization of diammonium copper disulphate hexahydrate single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Siva Sankari, R.; Perumal, Rajesh Narayana, E-mail: r.shankarisai@gmail.com

2014-03-01

Graphical abstract: Diammonium copper disulphate hexahydrate (DACS) is one of the most promising inorganic dielectric crystals with exceptional mechanical properties. Good quality crystals of DACS were grown by using solution method in a period of 30 days. The grown crystals were subjected to single crystal X-ray diffraction analysis in order to establish their crystalline nature. Thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis were performed for the crystal. Several solid state physical parameters have been determined for the grown crystals. The dielectric constant and the dielectric loss and AC conductivity of the grown crystal were studied as a functionmore » of frequency and temperature has been calculated and plotted. - Highlights: • Diammonium copper disulphate is grown for the first time and CCDC number obtained. • Thermal analysis is done to see the stability range of the crystals. • Band gap and UV cut off wavelength of the crystal are determined to be 2.4 eV and 472.86 nm, respectively. • Dielectric constant, dielectric loss and AC conductivity are plotted as a function of applied field. - Abstract: Diammonium copper disulphate hexahydrate is one of the most promising inorganic crystals with exceptional dielectric properties. A good quality crystal was harvested in a 30-day period using solution growth method. The grown crystal was subjected to various characterization techniques like single crystal X-ray diffraction analysis, thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis. Unit cell dimensions of the grown crystal have been identified from XRD studies. Functional groups of the title compounds have been identified from FTIR studies. Thermal stability of the samples was checked by TG/DTA studies. Band gap of the crystal was calculated. The dielectric constant and dielectric loss were studied as a function of frequency of the applied field. AC conductivity was plotted as a function of temperature.« less

Synthesis, crystal structure, thermal and nonlinear optical properties of new metal-organic single crystal: Tetrabromo (piperazinium) zincate (II) (TBPZ)

NASA Astrophysics Data System (ADS)

Boopathi, K.; Babu, S. Moorthy; Ramasamy, P.

2018-04-01

Tetrabromo (piperazinium) zincate, a new metal-organic crystal has been synthesized and its single crystal grown by slow evaporation method. The grown crystal has characterized by structural, spectral, thermal, linear and nonlinear optical properties. Single crystal X-ray diffractions study reveals that grown crystal belongs to orthorhombic crystal system with space group P212121. The presence of functional groups is identified by FT-IR spectral analysis. Thermal stability of the crystal was ascertained by TG-DTA measurement. The second order harmonic generation efficiency was measured using Kurtz and Perry technique and it was found to be 1.5 times that of KDP.

Studies on the growth, structural, spectral and third-order nonlinear optical properties of ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate single crystal.

PubMed

Silambarasan, A; Krishna Kumar, M; Thirunavukkarasu, A; Mohan Kumar, R; Umarani, P R

2015-01-25

An organic nonlinear optical bulk single crystal, Ammonium 3-carboxy-4-hydroxy benzenesulfonate monohydrate (ACHBS) was successfully grown by solution growth technique. Single crystal X-ray diffraction study confirms that, the grown crystal belongs to P21/c space group. Powder X-ray diffraction and high resolution X-ray diffraction analyses revealed the crystallinity of the grown crystal. Infrared spectral analysis showed the vibrational behavior of chemical bonds and its functional groups. The thermal stability and decomposition stages of the grown crystal were studied by TG-DTA analysis. UV-Visible transmittance studies showed the transparency region and cut-off wavelength of the grown crystal. The third-order nonlinear optical susceptibility of the grown crystal was estimated by Z-scan technique using He-Ne laser source. The mechanical property of the grown crystal was studied by using Vicker's microhardness test. Copyright © 2014 Elsevier B.V. All rights reserved.

Optical, mechanical and thermal behaviors of Nitrilotriacetic acid single crystal

NASA Astrophysics Data System (ADS)

Deepa, B.; Philominathan, P.

2017-11-01

An organic nonlinear single crystal of Nitrilotriacetic acid (NTAA) was grown for the first time by employing a simple slow evaporation technique. Single crystal X-ray diffraction (XRD) analysis reveals that the grown crystal belongs to the monoclinic system with noncentrosymmetric space group CC. Fourier transform infrared (FTIR) spectral study ascertains the presence of functional groups in NTAA. The molecular structure of the grown crystal was confirmed by Nuclear Magnetic Resonance (NMR) spectral analysis. The optical parameters such as transmittance, absorption coefficient and band gap were calculated from UV-Visible and fluorescence studies. Dielectric measurements were carried out for different frequency and temperature. The mechanical strength of the grown crystal was measured using Vickers microhardness test. The high thermal stability and the melting point of the grown crystal were also estimated using thermogravimetric (TGA) and differential thermal analyses (DTA). The confirmation of the grown crystals belonging to nonlinear optical crystals was performed by Kurtz-Perry technique and found as suitable candidate for optoelectronics applications.

Crystal structure and vibrational spectra of melaminium arsenate

NASA Astrophysics Data System (ADS)

Anbalagan, G.; Marchewka, M. K.; Pawlus, K.; Kanagathara, N.

2015-01-01

The crystals of the new melaminium arsenate (MAS) [C3H7N6+ṡH2AsO4-] were obtained by the slow evaporation of an aqueous solution at room temperature. Single crystal X-ray diffraction analysis reveals that the crystal belongs to triclinic system with centro symmetric space group P-1. The crystals are built up from single protonated melaminium residues and single dissociated arsenate H2AsO4- anions. The protonated melaminium ring is almost planar. A combination of ionic and donor-acceptor hydrogen-bond interactions linking together the melaminium and arsenate residues forms a three-dimensional network. Vibrational spectroscopic analysis is reported on the basis of FT-IR and FT-Raman spectra recorded at room temperature. Hydrogen bonded network present in the crystal gives notable vibrational effect. DSC has also been performed for the crystal shows no phase transition in the studied temperature range (113-293 K).

Growth and characterization of divalent transition metal ions doped zinc hydrogen phosphate single crystals

NASA Astrophysics Data System (ADS)

D'Souza, Delma; Jagannatha, N.; Nagaraja, K. P.; Rohith, P. S.; Pradeepkumar, K. V.

2018-05-01

Zinc hydrogen phosphate (ZnHP) single crystal co-doped with divalent transition metal ions Cobalt (Co2+) and Cadmium (Cd2+) is grown by gel technique in silica hydro gel media. The presence of Co2+ and Cd2+ dopants in the ZnHP crystal was confirmed by Energy Dispersive X-ray Analysis (EDAX).FTIR spectra of the grown crystal depict the stretching and bending vibration of PO4 units, water of crystallization and metal-oxygen bonds. Powder XRD analysis reveals that the grown crystal belongs to monoclinic system with spacegroup P 21. The thermal stability of the grown crystal is rectified from TG-DSC studies.

Growth, structural, optical, piezoelectric and etching analysis of L-lysine p-nitrophenolate monohydrate single crystals

NASA Astrophysics Data System (ADS)

Alexandar, A.; Lakshmanan, A.; Sakthy Priya, S.; Surendran, P.; Rameshkumar, P.

2017-09-01

Nonlinear optical single crystals of L-lysine p-nitrophenolate monohydrate (LLPNP) were grown in aqueous solution by the slow evaporation solution technique (SEST). The grown crystals were subjected to powder X-ray diffraction analysis, (PXRD) and it was found that the title compound was crystallized in the orthorhombic crystal system with noncentrosymmetric space group of P212121. The vibrational frequencies of various functional groups present in the crystal were analyzed using the FTIR spectrum with a wavenumber range between 450 cm-1 and 4000 cm-1. The microhardness analysis of the sample revealed that the crystal belongs to the soft material category. Piezoelectric analysis was performed to measure the value of the piezoelectric (d33) coefficient. Blue light emission of the material was confirmed using the photoluminescence spectrum. Thermal stability of the grown crystal was analyzed using a melting point apparatus and it was found that the LLPNP is stable upto 175∘C. Etching analysis was performed at various durations, in order to identify the surface properties of the LLPNP crystal.

Single Crystal Membranes

NASA Technical Reports Server (NTRS)

Stormont, R. W.; Morrison, A.

1974-01-01

Single crystal a- and c-axis tubes and ribbons of sodium beta-alumina and sodium magnesium beta-alumina were grown from sodium oxide rich melts. Additional experiments grew ribbon crystals containing sodium magnesium beta, beta double prime, beta triple prime, and beta quadruple prime. A high pressure crystal growth chamber, sodium oxide rich melts, and iridium for all surfaces in contact with the melt were combined with the edge-defined, film-fed growth technique to grow the single crystal beta-alumina tubes and ribbons. The crystals were characterized using metallographic and X-ray diffraction techniques, and wet chemical analysis was used to determine the sodium, magnesium, and aluminum content of the grown crystals.

Economic analysis of crystal growth in space

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Chung, A. M.; Yan, C. S.; Mccreight, L. R.

1972-01-01

Many advanced electronic technologies and devices for the 1980's are based on sophisticated compound single crystals, i.e. ceramic oxides and compound semiconductors. Space processing of these electronic crystals with maximum perfection, purity, and size is suggested. No ecomonic or technical justification was found for the growth of silicon single crystals for solid state electronic devices in space.

Anisotropy of nickel-base superalloy single crystals

NASA Technical Reports Server (NTRS)

Mackay, R. A.; Dreshfield, R. L.; Maier, R. D.

1980-01-01

The influence of orientation on the tensile and stress rupture behavior of 52 Mar-M247 single crystals was studied. Tensile tests were performed at temperatures between 23 and 1093 C; stress rupture behavior was examined between 760 and 1038 C. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factor contours for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The tensile properties correlated well with the appropriate Schmid factor contours. The stress rupture lives at lower testing temperatures were greatly influenced by the lattice rotations required to produce cross slip. A unified analysis was attained for the stress rupture life data generated for the Mar-M247 single crystals at 760 and 774 C under a stress of 724 MPa and the data reported for Mar-M200 single crystals tested at 760 C under a stress of 689 MPa. Based on this analysis, the stereographic triangle was divided into several regions which were rank ordered according to stress rupture life for this temperature regime.

Investigations on structural, optical, electrical, mechanical and third-order nonlinear behaviour of 3-aminopyridinium 2,4-dinitrophenolate single crystal

NASA Astrophysics Data System (ADS)

Mohanbabu, B.; Bharathikannan, R.; Siva, G.

2017-10-01

The single crystals of 3-aminopyridinium 2,4-dinitrophenolate (APDP) have been synthesized and grown by slow evaporation technique at room temperature. The crystal system was identified and lattice dimensions were measured from the single-crystal X-ray diffraction (SXRD) analysis. UV-visible absorption and transmittance spectra have been recorded in the region between 250 and 1100 nm. The different vibrational modes of the molecule were studied by Fourier transform infrared (FTIR) spectroscopic analysis. The decreasing tendency of dielectric constant with increasing frequency was analysed in dielectric study. The polarizability value calculated using Penn analysis well agrees with the value calculated using Clausius-Mossotti equation. The photoconductivity and photoluminescence behaviour were also studied on grown APDP crystal. The mechanical strength of the crystal has been studied using a Vickers' microhardness test. The stiffness constant and yield strength of the crystal were also calculated from the microhardness test. The third-order nonlinear optical parameters such as refractive index, absorption coefficient and third-order susceptibility were estimated by Z-scan studies.

Growth and studies of cyclohexylammonium 4-methoxy benzoate single crystal for nonlinear optical applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@annauniv.edu

2015-06-24

Cyclohexylammonium 4-Methoxy Benzoate (C4MB) was synthesised and the functional groups were confirmed by FTIR analysis. The purified C4MB (by repeated recrystallisation) was used for single crystal growth. Single crystal of cyclohexylammonium 4-methoxy benzoate was successfully grown by slow evaporation solution growth method at ambient temperature. Structural orientations were determined from single crystal X-ray diffractometer. Optical absorption and cut off wavelength were identified by UV-Visible spectroscopy. Thermal stability of the crystal was studied from thermogravimetric and differential thermal analyses curves. Mechanical stability of the grown crystal was analysed by Vicker’s microhardness tester. The Second Harmonic Generation (SHG) study revealed that themore » C4MB compound exhibits the SHG efficiency 3.3 times greater than KDP crystal.« less

Synthesis, crystal growth and characterization of bioactive material: 2- Amino-1H-benzimidazolium pyridine-3-carboxylate single crystal- a proton transfer molecular complex

NASA Astrophysics Data System (ADS)

Fathima, K. Saiadali; Kavitha, P.; Anitha, K.

2017-09-01

The 1:1 molecular adducts 2- Amino-1H-benzimidazolium pyridine-3-carboxylate (2ABPC) was synthesized and grown as single crystal where 2-aminobenzimidazole (ABI) acts as a donor and nicotinic acid (NA) acts as an acceptor. The presence of proton and carbon were predicted using 1H and 13C NMR spectral analysis. The molecular structure of the crystal was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R = 0.038 for 2469 reflections. The vibrational modes of functional group have been studied using FTIR and Raman spectroscopic analysis. The UV-Vis spectrum exhibited a visible band at 246 nm for 2ABPC due to the nicotinate anion of the molecule. Further, the antimicrobial activity of 2ABPC complex against B. subtilis, klebsiella pneumonia, Pseudomonas eruginos and E. coli pathogens was investigated. Minimum Inhibitory Concentration (MIC) for this crystal was obtained using UV spectrometer against MRSA pathogen. It was found that the benzimidazole with aminogroup at position 2 increases the general antimicrobial activities of 2ABPC crystal.

Growth, structural, optical, mechanical and quantum chemical analysis of unidirectional grown bis(guanidinium) 5-sulfosalicylate (BGSSA) single crystal

NASA Astrophysics Data System (ADS)

Sreedevi, R.; Saravana Kumar, G.; Amarsingh Bhabu, K.; Balu, T.; Murugakoothan, P.; Rajasekaran, T. R.

2018-02-01

Bis(guanidinium) 5-sulfosalicylate single crystal was grown by using Sankaranarayanan-Ramasamy (SR) method from the solution of methanol and water in equimolar ratio. Good quality crystal with 50 mm length and 10 mm in diameter was grown. The grown crystal was subjected to single crystal X-ray diffraction analysis to confirm the crystal structure and it was found to be orthorhombic. UV-Vis-NIR spectroscopic study revealed that the SR method grown crystal had good optical transparency with wide optical band gap of 4.4 eV. The presence of the functional groups and modes of vibrations were identified by FTIR spectroscopy recorded in the range 4000-400 cm-1. The mechanical strength of the grown crystal was confirmed using Vickers microhardness tester by applying load from 25 g to 100 g. Density functional theory (DFT) method with B3LYP/6-31-G (d,p) level basis set was employed and hence the optimized molecular geometry, first order hyperpolarizability, dipole moment, thermodynamic functions, molecular electrostatic potential and frontier molecular orbital analysis of the grown BGSSA sample was computed and analysed.

Growth and spectroscopic, thermodynamic and nonlinear optical studies of L-threonine phthalate crystal

NASA Astrophysics Data System (ADS)

Theras, J. Elberin Mary; Kalaivani, D.; Jayaraman, D.; Joseph, V.

2015-10-01

L-threonine phthalate (LTP) single crystal has been grown using a solution growth technique at room temperature. Single crystal X-ray diffraction analysis reveals that LTP crystallizes in monoclinic crystal system with space group C2/c. The optical absorption studies show that the crystal is transparent in the entire visible region with a cut-off wavelength 309 nm. The optical band gap is found to be 4.05 eV. The functional groups of the synthesized compound have been identified by FTIR spectral analysis. The functional groups present in the material were also confirmed by FT-RAMAN spectroscopy. Surface morphology and the presence of various elements were studied by SEM-EDAX analysis. The thermal stability of LTP single crystal has been analyzed by TGA/DTA studies. The thermodynamic parameters such as activation energy, entropy, enthalpy and Gibbs free energy were determined for the grown material using TG data and Coats-Redfern relation. Since the grown crystal is centrosymmetric, Z-Scan studies were carried out for analyzing the third order nonlinear optical property. The nonlinear absorption coefficient, nonlinear refractive index and susceptibility have been measured using Z-Scan technique.

Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

NASA Technical Reports Server (NTRS)

Arakere, N. K.; Swanson, G.

2002-01-01

High cycle fatigue (HCF) induced failures in aircraft gas turbine and rocket engine turbopump blades is a pervasive problem. Single crystal nickel turbine blades are being utilized in rocket engine turbopumps and jet engines throughout industry because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities over polycrystalline alloys. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493, PWA 1484, RENE' N-5 and CMSX-4. These alloys play an important role in commercial, military and space propulsion systems. Single crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant factor in the overall analysis. The failure modes of single crystal turbine blades are complicated to predict due to the material orthotropy and variations in crystal orientations. Fatigue life estimation of single crystal turbine blades represents an important aspect of durability assessment. It is therefore of practical interest to develop effective fatigue failure criteria for single crystal nickel alloys and to investigate the effects of variation of primary and secondary crystal orientation on fatigue life. A fatigue failure criterion based on the maximum shear stress amplitude /Delta(sub tau)(sub max))] on the 24 octahedral and 6 cube slip systems, is presented for single crystal nickel superalloys (FCC crystal). This criterion reduces the scatter in uniaxial LCF test data considerably for PWA 1493 at 1200 F in air. Additionally, single crystal turbine blades used in the alternate advanced high-pressure fuel turbopump (AHPFTP/AT) are modeled using a large-scale three-dimensional finite element model. This finite element model is capable of accounting for material orthotrophy and variation in primary and secondary crystal orientation. Effects of variation in crystal orientation on blade stress response are studied based on 297 finite element model runs. Fatigue lives at critical points in the blade are computed using finite element stress results and the failure criterion developed. Stress analysis results in the blade attachment region are also presented. Results presented demonstrates that control of secondary and primary crystallographic orientation has the potential to significantly increase a component S resistance to fatigue crack growth with- out adding additional weight or cost. [DOI: 10.1115/1.1413767

Growth, structural, optical and surface analysis of piperazinium tartrate: A NLO single crystal

NASA Astrophysics Data System (ADS)

Gupta, Apurva; Raseel Rahman M., K.; Nair, Lekha

2018-05-01

Single crystal of piperazinium tartrate (PPZT) was grown by the slow evaporation solution growth technique at room temperature. Crystallinity of grown crystal was examined by powder X-ray diffraction. High transparency and wide band gap were observed in the UV-Visible spectroscopic studies. Intense and broad emissions were observed in the blue region, as that is indicated by photoluminescence spectroscopy. The quality of the grown PPZT single crystals were analyzed by the etching studies using the water as the etchant.

Crystal growth, structural, optical, mechanical and thermal properties of a new nonlinear optical single crystal: L-Ornithine monohydrochloride.

PubMed

Balakrishnan, T; Ramamurthi, K

2009-03-01

Amino acid family crystals exhibit excellent nonlinear optical and electro optical properties. l-Ornithine monohydrochloride single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystals were characterized by single crystal and powder X-ray diffraction analysis, Fourier transform infrared (FTIR) spectroscopy, TGA, DTA and DSC analyses. UV-vis-NIR spectrum shows excellent transmission in the UV, visible and NIR region (300-1600nm). The mechanical properties of grown crystals were studied using Vickers microhardness tester. Its second harmonic generation efficiency was tested using Nd:YAG laser and is 1.25 times that of KDP.

Finite Element Analysis of a Copper Single Crystal Shape Memory Alloy-Based Endodontic Instruments

NASA Astrophysics Data System (ADS)

Vincent, Marin; Thiebaud, Frédéric; Bel Haj Khalifa, Saifeddine; Engels-Deutsch, Marc; Ben Zineb, Tarak

2015-10-01

The aim of the present paper is the development of endodontic Cu-based single crystal Shape Memory Alloy (SMA) instruments in order to eliminate the antimicrobial and mechanical deficiencies observed with the conventional Nickel-Titane (NiTi) SMA files. A thermomechanical constitutive law, already developed and implemented in a finite element code by our research group, is adopted for the simulation of the single crystal SMA behavior. The corresponding material parameters were identified starting from experimental results for a tensile test at room temperature. A computer-aided design geometry has been achieved and considered for a finite element structural analysis of the endodontic Cu-based single crystal SMA files. They are meshed with tetrahedral continuum elements to improve the computation time and the accuracy of results. The geometric parameters tested in this study are the length of the active blade, the rod length, the pitch, the taper, the tip diameter, and the rod diameter. For each set of adopted parameters, a finite element model is built and tested in a combined bending-torsion loading in accordance with ISO 3630-1 norm. The numerical analysis based on finite element procedure allowed purposing an optimal geometry suitable for Cu-based single crystal SMA endodontic files. The same analysis was carried out for the classical NiTi SMA files and a comparison was made between the two kinds of files. It showed that Cu-based single crystal SMA files are less stiff than the NiTi files. The Cu-based endodontic files could be used to improve the root canal treatments. However, the finite element analysis brought out the need for further investigation based on experiments.

Crystal growth and characterization of semi-organic 2-amino-5-nitropyridinium bromide (2A5NPBr) single crystals for third-order nonlinear optical (NLO) applications

NASA Astrophysics Data System (ADS)

Vediyappan, Sivasubramani; Arumugam, Raja; Pichan, Karuppasamy; Kasthuri, Ramachandran; Muthu, Senthil Pandian; Perumal, Ramasamy

2017-12-01

Semi-organic nonlinear optical (NLO) 2-amino-5-nitropyridinium bromide (2A5NPBr) single crystals have been grown by slow evaporation solution technique (SEST) with the growth period of 60 days. The single-crystal XRD analysis confirms the unit cell parameters of the grown crystal. The crystallinity of grown 2A5NPBr was analyzed by powder X-ray diffraction (PXRD) measurement. The presence of functional groups of 2A5NPBr crystal was confirmed by Fourier transform infrared (FTIR) spectrum analysis. The optical transmittance of the grown crystal was analyzed by UV-Vis-NIR analysis. It shows good transparency in the visible and NIR region and it is favorable for nonlinear optical (NLO) device applications. The chemical etching study was carried out and it reveals that the grown crystal has less dislocation density. The photoconductivity study reveals that the grown crystal possesses positive photoconductive nature. The thermal stability of the crystal has been investigated by thermogravimetric (TG) and differential thermal analysis (DTA). The dielectric constant and dielectric loss as a function of frequency were measured. The electronic polarizability (α) of 2A5NPBr molecule has been calculated theoretically by different ways such as Penn analysis, Clausius-Mossotti relation, Lorentz-Lorenz equation, optical bandgap, and coupled dipole method (CDM). The obtained values of electronic polarizability (α) are in good agreement with each other. Laser damage threshold (LDT) of 2A5NPBr crystal has been measured using Nd:YAG laser with the wavelength of 1064 nm. Third-order nonlinear optical property of the grown crystal was studied by Z-scan technique using He-Ne laser of wavelength 632.8 nm.

Crystal growth and characterization of semi organic nonlinear optical (NLO) piperazinium tetrachlorozincate monohydrate (PTCZ) single crystal

NASA Astrophysics Data System (ADS)

Karuppasamy, P.; Pandian, Muthu Senthil; Ramasamy, P.

2018-04-01

The semi-organic single crystal of piperazinium tetrachlorozincate monohydrate (PTCZ) was successfully grown by slow evaporation solution technique (SEST). The grown crystal was subjected to the single crystal XRD studies for confirming the unit cell parameters. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis and the optical band gap energy was calculated. The photoconductivity study reveals that the grown crystal has positive photoconductive nature. The mechanical stability of the grown crystal was analyzed using Vickers microhardness analyzer. The third-order nonlinear optical properties such as nonlinear refractive index (n2), absorption co-efficient (β) and susceptibility (χ(3)) were studied by Z-scan technique at 640 nm using solid state laser.

Bulk crystal growth and their effective third order nonlinear optical properties of 2-(4-fluorobenzylidene) malononitrile (FBM) single crystal

NASA Astrophysics Data System (ADS)

Priyadharshini, A.; Kalainathan, S.

2018-04-01

2-(4-fluorobenzylidene) malononitrile (FBM), an organic third order nonlinear (TONLO) single crystal with the dimensions of 32 × 7 × 11 mm3, has been successfully grown in acetone solution by slow evaporation technique at 35 °C. The crystal system (triclinic), space group (P-1) and crystalline purity of the titular crystal were measured by single crystal and powder X-ray diffraction, respectively. The molecular weight and the multiple functional groups of the FBM material were confirmed through the mass and FT-IR spectral analysis. UV-Vis-NIR spectral study enroles that the FBM crystal exhibits excellent transparency (83%) in the entire visible and near infra-red region with a wide bandgap 2.90 eV. The low dielectric constant (εr) value of FBM crystal is appreciable for microelectronics industry applications. Thermal stability and melting point (130.09 °C) were ascertained by TGA-DSC analysis. The laser-induced surface damage threshold (LDT) value of FBM specimen is found to be 2.14 GW/cm2, it is fairly good compared to other reported NLO crystals. The third - order nonlinear optical character of the FBM crystal was confirmed through the typical single beam Z-scan technique. All these finding authorized that the organic crystal of FBM is favorably suitable for NLO applications.

Crystal growth and characterization of third order nonlinear optical piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) single crystal

NASA Astrophysics Data System (ADS)

Pichan, Karuppasamy; Muthu, Senthil Pandian; Perumalsamy, Ramasamy

2017-09-01

The organic single crystal of piperazinium bis(4-hydroxybenzenesulphonate) (P4HBS) was grown by slow evaporation solution technique (SEST) at room temperature. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. Functional groups of P4HBS crystal were confirmed by FTIR spectrum analysis. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis. The grown crystal has good optical transmittance in the range of 410-1100 nm. In photoluminescence spectrum, sharp emission peaks are observed, which indicates the ultraviolet (UV) emission. The photoconductivity study reveals that the grown crystal has negative photoconductive nature. The thermal behaviour of the P4HBS crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). The mechanical stability of grown crystal was analyzed and the indentation size effect (ISE) was explained by Hays-Kendall's (HK) approach and proportional specimen resistance model (PSRM). Chemical etching study was carried out and the etch pit density (EPD) was calculated. The dielectric constant (ε‧) and dielectric loss (tan δ) as a function of frequency were measured for the grown crystal. The solid state parameters such as valence electron, plasma energy, Penn gap and Fermi energy were evaluated theoretically for the P4HBS using the empirical relation. The estimated values are used to calculate the electronic polarizability. The third-order nonlinear optical properties such as nonlinear refractive index (n2), absorption co-efficient (β) and susceptibility (χ(3)) were studied by Z-scan technique at 632.8 nm using He-Ne laser.

Transfiguring structural, optical and dielectric properties of cadmium thiourea acetate crystal by the addition of L-threonine for laser assisted device applications

NASA Astrophysics Data System (ADS)

Kulkarni, Rupali B.; Anis, Mohd; Hussaini, S. S.; Shirsat, Mahendra D.

2018-03-01

Present investigation reports the growth of pure and L-threonine (LT) doped cadmium thiourea acetate (CTA) crystals by slow solution evaporation technique followed by structural, optical and dielectric characterization studies. A bulk single crystal of LT-CTA has been grown at temperature 38 °C. The single crystal x-ray diffraction technique has been employed to confirm the structural parameters of pure and LT doped CTA crystals. The increase in optical transparency of LT-CTA crystal was ascertained in the range of 200 to 900 nm using UV-visible spectral analysis. The widened optical band gap of the LT-CTA crystal is found to be 4.7 eV. Pure and doped crystals are subjected to FT-IR analysis to indicate the presence of functional groups quantitatively. Appreciable enhancement in second harmonic generation (SHG) efficiency of LT-CTA crystal with reference to parent CTA was confirmed from Kurtz-Perry SHG test (1.31 times of CTA crystal). The assertive influence of LT on electrical properties of grown crystals has been investigated in the temperature range 35 °C-120 °C. Electronic purity and the color centered photoluminescence emission nature of pure and IA-CTA crystals were justified by luminescence analysis. With the aid of single beam Z-scan analysis, the Kerr lensing nonlinearity was identified and the magnitude of TONLO parameters has been determined. The cubic susceptibility (χ3) and figure of merit (FOM) was found to be 4.81 × 10-4esu and 978.35. Results vitalize LT-CTA for laser stabilization systems.

Growth and characterization of unidirectional benzil single crystal for photonic applications

NASA Astrophysics Data System (ADS)

Saranraj, A.; Thirupathy, J.; Dhas, S. Sahaya Jude; Jose, M.; Vinitha, G.; Dhas, S. A. Martin Britto

2018-06-01

Organic nonlinear optical benzil single crystal of fine quality with the dimensions of 168 × 14 mm2 was successfully grown in (100) plane from saturated solution by unidirectional SR method. The structural identity of the grown crystal was confirmed by powder XRD. High-resolution X-ray diffraction analysis indicates the crystalline perfection of the grown benzil crystal. The optical analysis was carried out by UV-visible spectroscopy which shows that the benzil crystal's cut off wavelength is 437 nm. The dielectric constant and dielectric loss of benzil crystal are found to be very much depending upon temperature and frequency. Ferroelectric nature of grown crystal was identified by P- E hysteresis analysis and to find the values of spontaneous polarization and coercive field. The laser damage threshold energy was studied with the help of Nd:YAG laser. The presence of third harmonic generation was identified by z-scan techniques.

Growth and characterization of hexamethylenetetramine crystals grown from solution

NASA Astrophysics Data System (ADS)

Babu, B.; Chandrasekaran, J.; Balaprabhakaran, S.

2014-06-01

Organic nonlinear optical single crystals of hexamethylenetetramine (HMT; 10 × 10 × 5 mm3) were prepared by crystallization from methanol solution. The grown crystals were subjected to various characterization techniques such as single crystal XRD, powder XRD, UV-Vis and electrical studies. Single crystal XRD analysis confirmed the crystalline structure of the grown crystals. Their crystalline nature was also confirmed by powder XRD technique. The optical transmittance property was identified from UV-Vis spectrum. Dielectric measurements were performed as a function of frequency at different temperatures. DC conductivity and photoconductivity studies were also carried out for the crystal. The powder second harmonic generation efficiency (SHG) of the crystal was measured using Nd:YAG laser and the efficiency was found to be two times greater than that of potassium dihydrogen phosphate (KDP).

Influence of bis-thiourea nickel nitrate on the structural, optical, electrical, thermal and mechanical behavior of a KDP single crystal for NLO applications

NASA Astrophysics Data System (ADS)

Rasal, Y. B.; Shaikh, R. N.; Shirsat, M. D.; Kalainathan, S.; Hussaini, S. S.

2017-03-01

A single crystal of bis-thiourea nickel nitrate (BTNN) doped potassium dihydrogen phosphate (KDP) has been grown from solution at room temperature by a slow evaporation technique. The cell parameters of the grown crystals were determined using single crystal x-ray diffraction analysis. The different functional groups of the grown crystal were confirmed using Fourier transform infrared analysis. The improved optical parameters of the grown crystal have been evaluated in the range of 200-900 nm using UV-visible spectral analysis. The grown crystal was transparent in the entire visible region and the band gap value was found to be 4.96 eV. The influence of BTNN on the third order nonlinear optical properties of KDP crystal has been investigated by means of the Z-scan technique. The second harmonic generation (SHG) efficiency of grown crystal measured using a Nd-YAG laser is 1.98 times higher than that of pure KDP. The third order nonlinear optical susceptibility (χ 3) and nonlinear absorption coefficient (β) of BTNN doped KDP crystal is found to be 1.77  ×  10-5 esu and 5.57  ×  10-6 cm W-1 respectively. The laser damage threshold (LDT) energy for the grown crystal has been measured by using a Q-switched Nd:YAG laser source. The bis-thiourea nickel nitrate shows authoritative impact on the dielectric properties of doped crystal. The influence of bis-thiourea nickel nitrate on the mechanical behavior of KDP crystal has been investigated using Vickers microhardness intender. The thermal behavior of BTNN doped KDP crystal has been analyzed by TGA/DTA analysis.

Efficient green luminescence of terbium oxalate crystals: A case study with Judd-Ofelt theory and single crystal structure analysis and the effect of dehydration on luminescence

NASA Astrophysics Data System (ADS)

Alexander, Dinu; Joy, Monu; Thomas, Kukku; Sisira, S.; Biju, P. R.; Unnikrishnan, N. V.; Sudarsanakumar, C.; Ittyachen, M. A.; Joseph, Cyriac

2018-06-01

Design and synthesis of Lanthanide based metal organic framework is a frontier area of research owing to their structural diversity enabling specific applications. The luminescence properties of rare earths, tuned by the structural features of Ln-MOFs are investigated extensively. Rare earth oxalates which can be synthesized in a facile method, ensuring the structural features of MOFs with excellent photoluminescence characteristics deserves much attention. This work is the first time report on the single crystal structure and Judd-Ofelt (JO) theoretical analysis - their correlation with the intense and sharp green luminescence of Terbium oxalate crystals. The intense green luminescence observed for Terbium oxalate crystals for a wide range of excitation from DUV to visible region despite the luminescence limiting factors are discussed. The absence of concentration quenching and lifting up of forbidden nature of f-f transitions, allowing direct excitation of Terbium ions is analysed with the help of JO theory and single crystal structure analysis. The JO analysis predicted the asymmetry of Terbium sites, allowing the electric dipole transitions and from the JO intensity parameters, promising spectroscopic parameters - emission cross section, branching ratio, gain band width and gain coefficient of the material were calculated. The single crystal structure analysis revealed the asymmetry of Tb sites and structure of Terbium oxalate is formed by the hydrogen bonded stacking of overlapped six Terbium membered rings connected by the oxalate ligands. The molecularly thick layers thus formed on the crystal surface are imaged by the atomic force microscopy. The presence of water channels in the structure and the effect of lattice water molecules on the luminescence intensity are also investigated.

Structural, mechanical, electrical and optical properties of a new lithium boro phthalate NLO crystal synthesized by a slow evaporation method

NASA Astrophysics Data System (ADS)

Mohanraj, K.; Balasubramanian, D.; Jhansi, N.

2017-11-01

A new non-linear optical (NLO) single crystal of lithium boro phthalate (LiBP) was grown by slow solvent evaporation technique. The powder sample was subjected to powder X-ray diffraction (PXRD) to find its crystalline nature and the crystal structure of the grown crystal was determined using single crystal X-ray (SXRD) diffraction analysis. The Fourier Transform Infrared (FTIR) spectrum was recorded for grown crystal to identify the various functional groups present in the compound. The mechanical property of the LiBP single crystal was studied using Vickers microhardness tester. The dielectric constant and dielectric loss measurements were carried out for the grown crystal at various temperatures. The grown crystal was subjected to UV-Visible Spectral Studies to analyze the linear optical behavior of the grown crystal. The Kurtz-Perry Powder technique was employed to measure the Second Harmonic Generation efficiency of the grown crystal.

Crucial role of molecular planarity on the second order nonlinear optical property of pyridine based chalcone single crystals

NASA Astrophysics Data System (ADS)

Menezes, Anthoni Praveen; Jayarama, A.; Ng, Seik Weng

2015-05-01

An efficient nonlinear optical material 2E-3-(4-bromophenyl)-1-(pyridin-3-yl) prop-2-en-1-one (BPP) was synthesized and single crystals were grown using slow evaporation solution growth technique at room temperature. Grown crystal had prismatic morphology and its structure was confirmed by various spectroscopic studies, elemental analysis, and single crystal X-ray diffraction (XRD) technique. The single crystal XRD of the crystal showed that BPP crystallizes in monoclinic system with noncentrosymmetric space group P21 and the cell parameters are a = 5.6428(7) Å, b = 3.8637(6) Å, c = 26.411(2) Å, β = 97.568(11) deg and v = 575.82(12) Å3. The UV-Visible spectrum reveals that the crystal is optically transparent and has high optical energy band gap of 3.1 eV. The powder second harmonic generation efficiency (SHG) of BPP is 6.8 times that of KDP. From thermal analysis it is found that the crystal melts at 139 °C and decomposes at 264 °C. High optical transparency down to blue region, higher powder SHG efficiency and better thermal stability than that of urea makes this chalcone derivative a promising candidate for SHG applications. Furthermore, effect of molecular planarity on SHG efficiency and role of pyridine ring adjacent to carbonyl group in forming noncentrosymmetric crystal systems of chalcone family is also discussed.

Investigations on synthesis, growth and physicochemical properties of semi-organic NLO crystal bis(thiourea) ammonium nitrate for nonlinear frequency conversion

NASA Astrophysics Data System (ADS)

Anbarasi, A.; Ravi Kumar, S. M.; Sundar, G. J. Shanmuga; Mosses, M. Allen; Raj, M. Packiya; Prabhakaran, M.; Ravisankar, R.; Gunaseelan, R.

2017-10-01

Bis(thiourea) ammonium nitrate (BTAN), a new nonlinear optical crystal was grown successfully by slow evaporation technique using water as solvent at room temperature. The grown crystals were optically good quality with dimensions upto 10 × 6 × 3 mm3. Single crystal X-Ray diffraction analysis reveals that the crystal lattice is orthorhombic. From Powder X-ray diffraction analysis the diffraction planes have been indexed. The presence of the various functional groups of BTAN was identified through FTIR spectroscopic analysis. UV cut-off wavelength was observed from optical absorbance spectrum and it was found to be 240 nm. Second harmonic efficiency was determined using Kurtz powder method in comparison with KDP to confirm the nonlinearity of the material. Thermal analysis confirmed that grown crystal is thermally stable upto 184 °C. Microhardness studies show that hardness number (Hv) increases with load. Conductivity measurements such as dielectric, ac and photoconductivity were studied. Growth mechanism and surface features of the as grown single crystal was analysed by chemical etching analysis.

Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

NASA Astrophysics Data System (ADS)

Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

2015-01-01

Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

Phase transitions of antibiotic clarithromycin forms I, IV and new form VII crystals.

PubMed

Ito, Masataka; Shiba, Rika; Watanabe, Miteki; Iwao, Yasunori; Itai, Shigeru; Noguchi, Shuji

2018-06-01

Metastable crystal form I of the antibiotic clarithromycin has a pharmaceutically valuable characteristic that its crystalline phase transition can be applied for its sustained release from tablets. The phase transition of form I was investigated in detail by single crystal and powder X-ray analyses, dynamic vapor sorption analysis and thermal analysis. The single crystal structure of form I revealed that form I was not an anhydrate crystal but contained a partially occupied water molecule in the channel-like void space. Dynamic vapor sorption (DVS) analysis demonstrated that form I crystals reversibly sorbed water molecules in two steps when the relative humidity (RH) increased and finally transited to hydrate form IV at 95% RH. DVS analysis also showed that when the RH decreased form IV crystals lost water molecules at 40% RH and transited to the newly identified anhydrate crystal form VII. Form VII reversibly transited to form IV at lower RH than form I, suggesting that form I is more suitable for manufacturing a sustained-release tablet of CAM utilizing the crystalline phase transition. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis, growth, structure and nonlinear optical properties of a semiorganic 2-carboxy pyridinium dihydrogen phosphate single crystal

NASA Astrophysics Data System (ADS)

Nagapandiselvi, P.; Baby, C.; Gopalakrishnan, R.

2015-09-01

A new semiorganic compound namely, 2-carboxy pyridinium dihydrogen phosphate (2CPDP) was synthesised and grown as single crystals by slow evaporation solution growth technique. Single crystal XRD showed that 2CPDP belongs to monoclinic crystal system with space group P21/n. The molecular structure was further confirmed by modern spectroscopic techniques like FT-NMR (1H, 13C &31P), FT-IR, UV-Vis-NIR and Fluorescence. The UV-Vis-NIR analysis revealed suitability of the crystal for nonlinear optical applications. The photo active nature of the material is established from fluorescence studies. TG-DSC analysis showed that 2CPDP was thermally stable up to 170 °C. The dependence of dielectric properties on frequency and temperature were also studied. Nonlinear optical absorption determined from open aperture Z-Scan analysis by employing picosecond Nd-YAG laser, revealed that 2CPDP can serve as a promising candidate for optical limiting applications.

Crystalline perfection, optical and piezoelectric properties of a novel semi-organic single crystal: Zinc guanidinium sulphate

NASA Astrophysics Data System (ADS)

Nandhini, S.; Murugakoothan, P.

2018-04-01

Zinc Guanidinium Sulfate (ZGuS), a semi-organic single crystal, was synthesized using slow evaporation solution growth technique. It is a non-centrosymmetric crystal with space group I4 ¯2d . The crystalline nature of the crystal and the strain were determined using powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was revealed using HR-XRD analysis. The UV-vis-NIR transmittance spectrum depicts 60% transparency with lower-cut off wavelength of 210 nm. The emission spectrum of the crystal was determined using photoluminescence study. Piezoelectricity was confirmed by determining the piezoelectric charge coefficient (d33). These findings shows that the title compound can be employed for photonic and transducer applications.

Study on structural, morphological, optical and thermal properties of guanidine carbonate doped nickel sulfate hexahydrate crystal.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2015-01-05

The single crystal of guanidine carbonate doped nickel sulfate hexahydrate was grown from solution for ultraviolet filters. The single crystal XRD confirms that the grown single crystal belongs to the tetragonal system with the space group of P4₁2₁2. The crystallinity of the grown crystal was estimated by powder X-ray diffraction studies. The optical transmission and thermal stability of as-grown guanidine carbonate doped nickel sulfate single crystals have been studied. The optical transmission spectrum demonstrates the characteristics of ultraviolet filters. The TG/DTA studies confirm the thermal properties of grown crystals. Thermo-gravimetric analysis showed that the dehydration temperature of the guanidine carbonate doped nickel sulfate crystal is about 100 °C, which is much higher than that of pure nickel sulfate hexahydrate (NSH) crystals which is 72 °C. The growth behaviors and dislocation density were detected under the high resolution XRD and etching studies respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Investigation on the growth and characterization of 4-aminobenzophenone single crystal by the vertical dynamic gradient freeze technique

NASA Astrophysics Data System (ADS)

Prabhakaran, SP.; Ramesh Babu, R.; Sukumar, M.; Bhagavannarayana, G.; Ramamurthi, K.

2014-03-01

Growth of bulk single crystal of 4-Aminobenzophenone (4-ABP) from the vertical dynamic gradient freeze (VDGF) setup designed with eight zone furnace was investigated. The experimental parameters for the growth of 4-ABP single crystal with respect to the design of VDGF setup are discussed. The eight zones were used to generate multiple temperature gradients over the furnace, and video imaging system helped to capture the real time growth and solid-liquid interface. 4-ABP single crystal with the size of 18 mm diameter and 40 mm length was grown from this investigation. Structural and optical quality of grown crystal was examined by high resolution X-ray diffraction and UV-visible spectral analysis, respectively and the blue emission was also confirmed from the photoluminescence spectrum. Microhardness number of the crystal was estimated at different loads using Vicker's microhardness tester. The size and quality of single crystal grown from the present investigation are compared with the vertical Bridgman grown 4-ABP.

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aravinth, K., E-mail: anandcgc@gmail.com; Babu, G. Anandha, E-mail: anandcgc@gmail.com; Ramasamy, P., E-mail: anandcgc@gmail.com

2014-04-24

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

Crystallization of toxic glycol solvates of rifampin from glycerin and propylene glycol contaminated with ethylene glycol or diethylene glycol.

PubMed

de Villiers, Melgardt M; Caira, Mino R; Li, Jinjing; Strydom, Schalk J; Bourne, Susan A; Liebenberg, Wilna

2011-06-06

This study was initiated when it was suspected that syringe blockage experienced upon administration of a compounded rifampin suspension was caused by the recrystallization of toxic glycol solvates of the drug. Single crystal X-ray structure analysis, powder X-ray diffraction, thermal analysis and gas chromatography were used to identify the ethylene glycol in the solvate crystals recovered from the suspension. Controlled crystallization and solubility studies were used to determine the ease with which toxic glycol solvates crystallized from glycerin and propylene glycol contaminated with either ethylene or diethylene glycol. The single crystal structures of two distinct ethylene glycol solvates of rifampin were solved while thermal analysis, GC analysis and solubility studies confirmed that diethylene glycol solvates of the drug also crystallized. Controlled crystallization studies showed that crystallization of the rifampin solvates from glycerin and propylene glycol depended on the level of contamination and changes in the solubility of the drug in the contaminated solvents. Although the exact source of the ethylene glycol found in the compounded rifampin suspension is not known, the results of this study show how important it is to ensure that the drug and excipients comply with pharmacopeial or FDA standards.

Synthesis, growth and characterization of L-Phenylalaninium methanesulfonate nonlinear optical single crystal

NASA Astrophysics Data System (ADS)

Mangaiyarkarasi, K.; Ravichandran, A. T.; Anitha, K.; Manivel, A.

2018-03-01

The titled compound, L-Phenylalaninium methanesulfonate (LPA-MS) was synthesized and grown into single crystals by slow solvent evaporation solution growth technique in aqueous solution containing equimolar concentrations of L-phenylalanine and methanesulfonic acid at room temperature. The grown crystals were subjected to single crystal X-ray diffraction studies. It crystallizes in the monoclinic crystal structure with P21 space group and the unit cell parameters are a = 5.312 (10) Å, b = 8.883 (2) Å and c = 25.830 (7) Å. The functional groups of the LPA-MS crystal were confirmed with FT-IR and FT-Raman analysis. The carbon-hydrogen skeleton was confirmed with 1H NMR and 13C NMR analysis. TG-DTG and DSC studies were carried out to determine the thermal stability of the crystals. The optical transparency ranges were studied through UV-vis-spectroscopy and the crystal was found to be transparent in the visible region. The second Harmonic generation (SHG) efficiency of the grown LPA-MS crystal was measured by the Kurtz-Perry powder technique. The dipolar nature of the L-phenylalaninium methanesulfonate and the presence of the intermolecular hydrogen bonding between the molecules are the vital factors responsible for the existence of SHG activity in the crystal.

Synthesis, structural, optical and thermal properties of N-methyl-N-aryl benzamide organic single crystals grown by a slow evaporation technique

NASA Astrophysics Data System (ADS)

Prabukanthan, P.; Lakshmi, R.; Harichandran, G.; Kumar, C. Sudarsana

2018-03-01

The organic materials, N-methyl-N-aryl benzamides were synthesized from benzoylation of N-methyl-4-nitrobenzenamine (MNBA) using suitably substituted benzoyl chlorides. The products were purified by recrystallization and their single crystal were grown by a slow evaporation technique. The crystals were characterized by FTIR, UV-Vis-NIR, 1H &13C NMR, and single & powder X-ray diffraction. Thermal stability of the crystals was studied by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric and NLO properties of MNPB, FMNPB and MMNPB crystals were studied. The second harmonic generation (SHG) has been confirmed by the Kurtz powder test for all these crystals and the SHG efficiency of MMNPB crystal was found to be 2.25 times higher than that of KDP crystal.

Structural and optical properties of WTe2 single crystals synthesized by DVT technique

NASA Astrophysics Data System (ADS)

Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

2018-05-01

Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

Thermal, mechanical, optical and conductivity studies of a novel NLO active L-phenylalanine L-phenylalaninium dihydrogenphosphate single crystal

NASA Astrophysics Data System (ADS)

Sujatha, T.; Cyrac Peter, A.; Vimalan, M.; Merline Shyla, J.; Madhavan, J.

2010-08-01

An efficient, novel, semi-organic, nonlinear optical (NLO) material L-phenylalanine L-phenylalaninium dihydrogenphosphate (LPADHP), single crystal of dimension 11×5×2 mm 3, has been grown by the slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to monoclinic system with the space group P2 1. The functional groups present in the crystal were confirmed by the Fourier transform infrared technique. Optical absorption spectrum shows that the material possesses very low absorption in the entire visible region. Thermal analysis confirmed that the crystal is thermally stable up to 161 °C. The frequency dependent dielectric properties of the grown crystal were studied for various temperatures. The second harmonic generation (SHG) efficiency of the grown crystal is 1.2 times greater than that of the potassium dihydrogenphosphate (KDP) single crystal. The laser induced surface damage threshold for the grown crystal was found to be 6.3 GW cm -2 with Nd:YAG laser assembly AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

Synthesis, crystal growth, structural, thermal, optical and mechanical properties of solution grown 4-methylpyridinium 4-hydroxybenzoate single crystal.

PubMed

Sudhahar, S; Krishna Kumar, M; Sornamurthy, B M; Mohan Kumar, R

2014-01-24

Organic nonlinear optical material, 4-methylpyridinium 4-hydroxybenzoate (4MPHB) was synthesized and single crystal was grown by slow evaporation solution growth method. Single crystal and powder X-ray diffraction analyses confirm the structure and crystalline perfection of 4MPHB crystal. Infrared, Raman and NMR spectroscopy techniques were used to elucidate the functional groups present in the compound. TG-DTA analysis was carried out in nitrogen atmosphere to study the decomposition stages, endothermic and exothermic reactions. UV-visible and Photoluminescence spectra were recorded for the grown crystal to estimate the transmittance and band gap energy respectively. Linear refractive index, birefringence, and SHG efficiency of the grown crystal were studied. Laser induced surface damage threshold and mechanical properties of grown crystal were studied to assess the suitability of the grown crystals for device applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Modified Bridgman-Stockbarger growth and characterization of LiInSe{sub 2} single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vijayakumar, P., E-mail: ramasamyp@ssn.edu.in; Magesh, M., E-mail: ramasamyp@ssn.edu.in; Arunkumar, A., E-mail: ramasamyp@ssn.edu.in

2014-04-24

The LiInSe{sub 2} polycrystalline materials were successfully synthesized from melt and temperature oscillation method. 8 mm diameter and 32 mm length single crystal was grown from Bridgman-Stockbarger method with steady ampoule rotation. Crystalline phase was confirmed by powder XRD pattern. Thermo gravimetric and differential thermal analysis confirms that the melting point of the grown crystal is 897°C. Rutherford backscattering analysis (RBS) gives the crystal composition as Li{sub 0.8}In{sub 1.16}Se{sub 2.04}. The crystalline perfection of the grown crystal was analyzed by High resolution X-ray diffraction measurements (HRXRD). The electrical properties of the grown crystal were analyzed by Hall effect measurements andmore » it confirms the n-type semiconducting nature.« less

Study of structural and optical properties of YAG and Nd:YAG single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kostić, S.; Lazarević, Z.Ž., E-mail: lzorica@yahoo.com; Radojević, V.

2015-03-15

Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. Themore » critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.« less

Orientation dependence of the stress rupture properties of Nickel-base superalloy single crystals

NASA Technical Reports Server (NTRS)

Mackay, R. A.

1981-01-01

The influence of orientation of the stress rupture behavior of Mar-M247 single crystals was studied. Stress rupture tests were performed at 724 MPa and 774 C where the effect of anisotropy is prominent. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factors for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The stress rupture lives were found to be greatly influenced by the lattice rotations required to produce intersecting slip, because steady-state creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited a large primary creep strain, a large effective stress level at the onset of steady-state creep, and consequently a short stress rupture life. A unified analysis was attained for the stress rupture behavior of the Mar-M247 single crystals tested in this study at 774 C and that of the Mar-M200 single crystals tested in a prior study at 760 C. In this analysis, the standard 001-011-111 stereographic triangle was divided into several regions of crystallographic orientation which were rank ordered according to stress rupture life for this temperature regime. This plot indicates that those crystals having orientations within about 25 deg of the 001 exhibited significantly longer lives when their orientations were closer to the 001-011 boundary of the stereographic triangle than to the 001-111 boundary.

Synthesis, growth, structural, thermal and optical studies of pyrrolidinium-2-carboxylate-4-nitrophenol single crystals.

PubMed

Swarna Sowmya, N; Sampathkrishnan, S; Vidyalakshmi, Y; Sudhahar, S; Mohan Kumar, R

2015-06-15

Organic nonlinear optical material, pyrrolidinium-2-carboxylate-4-nitrophenol (PCN) was synthesized and single crystals were grown by slow evaporation solution growth method. Single crystal X-ray diffraction analysis confirmed the structure and lattice parameters of PCN crystals. Infrared, Raman and NMR spectral analyses were used to elucidate the functional groups present in the compound. The thermal behavior of synthesized compound was studied by thermogravimetric and differential scanning calorimetry (TG-DSC) analyses. The photoluminescence property was studied by exciting the crystal at 360 nm. The relative second harmonic generation (SHG) efficiency of grown crystal was estimated by using Nd:YAG laser with fundamental wavelength of 1,064 nm. Copyright © 2015 Elsevier B.V. All rights reserved.

Analytical studies on the crystal melt interface shape in the Czochralski process for oxide single crystals

NASA Astrophysics Data System (ADS)

Jeong, Ja Hoon; Kang, In Seok

2000-09-01

Effects of the operating conditions on the crystal-melt interface shape are analytically investigated for the Czochralski process of the oxide single crystals. The ideas, which were used for the silicon single-crystal growth by Jeong et al. (J. Crystal Growth 177 (1997) 157), are extended to the oxide single-crystal growth problem by considering the internal radiation in the crystal phase and the melt phase heat transfer with the high Prandtl number. The interface shape is approximated in the simplest form as a quadratic function of radial position and an expression for the deviation from the flat interface shape is derived as a function of operating conditions. The radiative heat transfer rate between the interface and the ambient is computed by calculating the view factors for the curved interface shape with the assumption that the crystal phase is completely transparent. For the melt phase, the well-known results from the thermal boundary layer analysis are applied for the asymptotic case of high Prandtl number based on the idea that the flow field near the crystal-melt interface can be modeled as either a uniaxial or a biaxial flow. Through this work, essential information on the interface shape deformation and the effects of operating conditions are brought out for the oxide single-crystal growth.

Crystal structure, spectral, thermal and dielectric studies of a new zinc benzoate single crystal

NASA Astrophysics Data System (ADS)

Bijini, B. R.; Prasanna, S.; Deepa, M.; Nair, C. M. K.; Rajendra Babu, K.

2012-11-01

Single crystals of zinc benzoate with a novel structure were grown in gel media. Sodium metasilicate of gel density 1.04 g/cc at pH 6 was employed to yield transparent single crystals. The crystal structure of the compound was ascertained by single crystal X-ray diffractometry. It was noted that the crystal belongs to monoclinic system with space group P21/c with unit cell parameters a = 10.669(1) Å, b = 12.995(5) Å, c = 19.119(3) Å, and β = 94.926(3)°. The crystal was seen to possess a linear polymeric structure along b-axis; with no presence of coordinated or lattice water. CHN analysis established the stoichiometric composition of the crystal. The existence of functional groups present in the single crystal system was confirmed by FT-IR studies. The thermal characteristic of the sample was analysed by TGA-DTA techniques, and the sample was found to be thermally stable up to 280 °C. The kinetic and thermodynamic parameters were also determined. UV-Vis spectroscopy corroborated the transparency of the crystal and revealed the optical band gap to be 4 eV. Dielectric studies showed decrease in the dielectric constant of the sample with increase in frequency.

Fretting Stresses in Single Crystal Superalloy Turbine Blade Attachments

NASA Technical Reports Server (NTRS)

Arakere, Nagaraj K.; Swanson, Gregory

2000-01-01

Single crystal nickel base superalloy turbine blades are being utilized in rocket engine turbopumps and turbine engines because of their superior creep, stress rupture, melt resistance and thermomechanical fatigue capabilities over polycrystalline alloys. Currently the most widely used single crystal nickel base turbine blade superalloys are PWA 1480/1493 and PWA 1484. These alloys play an important role in commercial, military and space propulsion systems. High Cycle Fatigue (HCF) induced failures in aircraft gas turbine and rocket engine turbopump blades is a pervasive problem. Blade attachment regions are prone to fretting fatigue failures. Single crystal nickel base superalloy turbine blades are especially prone to fretting damage because the subsurface shear stresses induced by fretting action at the attachment regions can result in crystallographic initiation and crack growth along octahedral planes. Furthermore, crystallographic crack growth on octahedral planes under fretting induced mixed mode loading can be an order of magnitude faster than under pure mode I loading. This paper presents contact stress evaluation in the attachment region for single crystal turbine blades used in the NASA alternate Advanced High Pressure Fuel Turbo Pump (HPFTP/AT) for the Space Shuttle Main Engine (SSME). Single crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant factor in the overall analysis. Blades and the attachment region are modeled using a large-scale 3D finite element (FE) model capable of accounting for contact friction, material orthotrophy, and variation in primary and secondary crystal orientation. Contact stress analysis in the blade attachment regions is presented as a function of coefficient of friction and primary and secondary crystal orientation, Stress results are used to discuss fretting fatigue failure analysis of SSME blades. Attachment stresses are seen to reach peak values at locations where fretting cracks have been observed. Fretting stresses at the attachment region are seen to vary significantly as a function of crystal orientation. Attempts to adapt techniques used for estimating fatigue life in the airfoil region, for life calculations in the attachment region, are presented. An effective model for predicting crystallographic crack initiation under mixed mode loading is required for life prediction under fretting action.

Growth, optical, thermal, mechanical and dielectric studies of sodium succinate hexahydrate (β phase) single crystal: A promising third order NLO material

NASA Astrophysics Data System (ADS)

Mageshwari, P. S. Latha; Priya, R.; Krishnan, S.; Joseph, V.; Das, S. Jerome

2016-11-01

A third order nonlinear optical (NLO)single crystals of sodium succinate hexahydrate (SSH) (β phase) has been grown by a slow evaporation growth technique using aqueous solution at ambient temperature. The lattice parameters and morphology of SSH were determined by single crystal X-ray diffraction analysis. SSH crystallizes in centrosymmetric monoclinic system with space group P 21 / c and the crystalline purity was analyzed by powder X-ray diffraction analysis. The UV-vis-NIR spectrum reveals that the crystal is transparent in the entire visible region. The recorded FT-IR spectrum verified the presence of various functional groups in the material. NMR analysis of the grown crystal confirms the structural elucidation and detects the major and minor functional groups present in the title compound. ICP-OES analysis proved the presence of sodium in SSH. TG-DTA/DSCanalysis was used to investigate the thermal stability of the material. The dielectric permittivity and dielectric loss of SSH were carried out as a function of frequency for different temperatures and the results were discussed. The mechanical stability was evaluated from Vicker's microhardness test. The third order nonlinear optical properties of SSH has been investigated employing Z-scan technique with He-Ne laser operating at 632.8 nm wavelength.

Synthesis, growth, structural, spectral, thermal, chemical etching, linear and nonlinear optical and mechanical studies of an organic single crystal 4-chloro 4-nitrostilbene (CONS): a potential NLO material.

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-07-01

4-Chloro 4-nitrostilbene (CONS) a new organic nonlinear optical material has been synthesized. Employing slow evaporation method, good optical quality single crystals (dimensions up to 6×2×3 mm(3)) have been grown using ethyl methyl ketone (EMK) as a solvent. The grown crystals have been subjected to various characterizations such as single crystal X-ray diffraction, powder XRD, Fourier Transform Infrared spectroscopy (FTIR), proton NMR, solid UV absorption, SHG studies. Single crystal X-ray diffraction reveals that the crystal system belongs to monoclinic with noncentrosymmetric space group P21. The UV-Vis absorption spectrum has been recorded and found that the cut off wavelength is 380 nm. Functional groups and the structure of the title compound have been confirmed by FTIR and (1)H NMR spectroscopic analyses respectively. Molecular mass of the CONS confirmed by the high resolution mass spectral analysis .The thermal behavior of the grown crystal has been studied by TG/DTA analysis and it shows the melting point is at 188.66 °C. Dislocations and growth pattern present in the grown crystal revealed by the etching study. The mechanical strength of the CONS crystal has been studied by Vicker's hardness measurement. The SHG efficiency of the grown crystal has been determined by Kurtz and Perry powder test which revealed that the CONS crystal (327 mV) has 15 times greater efficiency than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis, high-resolution NMR spectroscopic analysis, and single-crystal X-ray diffraction of isoxazoline tetracycles.

PubMed

Fascio, Mirta L; Alvarez-Larena, Angel; D'Accorso, Norma B

2002-11-29

Three isoxazoline tetracycles were obtained enantiomerically pure by intramolecular 1,3-dipolar cycloaddition. The characterization of the new compounds was performed by high-resolution 1H and 13C NMR spectroscopy. The relative configuration of the new chiral centers was determined by NOESY experiments and confirmed by single-crystal X-ray structural analysis.

Dry-growth of silver single-crystal nanowires from porous Ag structure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Chuantong, E-mail: chenchuantong@sanken.osaka-u.ac.jp; Nagao, Shijo; Jiu, Jinting

A fabrication method of single crystal Ag nanowires in large scale is introduced without any chemical synthesis in wet processes, which usually generates fivefold twinned nanowires of fcc metals. Dense single-crystal nanowires grow on a mechanically polished surface of micro-porous Ag structure, which is created from Ag micro-particles. The diameter and the length of the nanowires can be controlled simply by changing the temperature and the time of the heating during the nanowire growth in air. Unique growth mechanism is described in detail, based on stress-induced migration accelerated by the micro-porous structure where the origin of Ag nanowires growth ismore » incubated. Transmission electron microscopy analysis on the single crystal nanowires is also presented. This simple method offered an alternative preparation for metallic nanowires, especially with the single crystal structure in numerous applications.« less

Growth of L-Valinium Aluminium Chloride single crystal for OLED and super-capacitor applications

NASA Astrophysics Data System (ADS)

Kalaivani, D.; Vijayalakshmi, S.; Theras, J. Elberin Mary; Jayaraman, D.; Joseph, V.

2015-12-01

L-Valinium Aluminium Chloride (LVAC), a novel semi-organic material, was grown using slow evaporation under isothermal condition. The single crystal data reveal that the grown crystal belongs to monoclinic system. The SEM micrographs give clear picture about the surface morphology. Further, they confirm the inclusion of aluminium chloride into atomic sites of L-Valine. The compositional elements present in the crystal were identified through EDAX analysis. The mass spectral analysis was carried out to determine the molecular weight of the grown crystal. The optical transparency of the grown crystal was investigated by UV-vis-NIR spectrum. FTIR spectral study was used to identify the functional groups present in the grown material. The luminescence characteristics of grown material were analysed to confirm the effect of metal ion on the ligand. This property makes the material suitable for OLED application. The supercapacitive performance of the grown crystal was finally studied using cyclic voltammetry.

Reliability analysis of single crystal NiAl turbine blades

NASA Technical Reports Server (NTRS)

Salem, Jonathan; Noebe, Ronald; Wheeler, Donald R.; Holland, Fred; Palko, Joseph; Duffy, Stephen; Wright, P. Kennard

1995-01-01

As part of a co-operative agreement with General Electric Aircraft Engines (GEAE), NASA LeRC is modifying and validating the Ceramic Analysis and Reliability Evaluation of Structures algorithm for use in design of components made of high strength NiAl based intermetallic materials. NiAl single crystal alloys are being actively investigated by GEAE as a replacement for Ni-based single crystal superalloys for use in high pressure turbine blades and vanes. The driving force for this research lies in the numerous property advantages offered by NiAl alloys over their superalloy counterparts. These include a reduction of density by as much as a third without significantly sacrificing strength, higher melting point, greater thermal conductivity, better oxidation resistance, and a better response to thermal barrier coatings. The current drawback to high strength NiAl single crystals is their limited ductility. Consequently, significant efforts including the work agreement with GEAE are underway to develop testing and design methodologies for these materials. The approach to validation and component analysis involves the following steps: determination of the statistical nature and source of fracture in a high strength, NiAl single crystal turbine blade material; measurement of the failure strength envelope of the material; coding of statistically based reliability models; verification of the code and model; and modeling of turbine blades and vanes for rig testing.

Growth of single crystalline delafossite LaCuO2 by the travelling-solvent floating zone method

NASA Astrophysics Data System (ADS)

Mohan, A.; Büchner, B.; Wurmehl, S.; Hess, C.

2014-09-01

Single crystals of LaCuO2 have been grown for the first time using the travelling-solvent floating zone method. The crystal was grown in an Ar-atmosphere by reduction of La2Cu2O5, which was used as the feed rod composition for the growth. The grown crystal has been characterized with regard to phase purity and single crystallinity using powder X-ray diffraction, energy dispersive X-ray analysis, Laue diffraction and scanning electron microscopy.

Optical Properties of Natural Minerals in the Far-Infrared

NASA Astrophysics Data System (ADS)

Long, Larry Lavern

The reflectivity of natural mineral powders were measured in the far infrared. The complex indices of refraction were then determined by Kramers-Kronig analysis or dispersive analysis. The samples were constructed by pressing the powdered sample into a 13 mm diameter pellet. A few of the samples that were measured were kaolin, illite, and montmorillonite, clay samples that could not be obtained in large single crystals. For calcite and gypsum crystals a comparison between the single crystal measurements and powder measurements was done to determine the effect of sample preparation on the measured spectra.

Analysis of rapidly synthesized guest-filled porous complexes with synchrotron radiation: Practical guidelines for the crystalline sponge method

DOE PAGES

Ramadhar, Timothy R.; Zheng, Shao -Liang; Chen, Yu -Sheng; ...

2015-01-01

A detailed set of synthetic and crystallographic guidelines for the crystalline sponge method based upon the analysis of expediently synthesized crystal sponges using third-generation synchrotron radiation are reported. The procedure for the synthesis of the zinc-based metal–organic framework used in initial crystal sponge reports has been modified to yield competent crystals in 3 days instead of 2 weeks. These crystal sponges were tested on some small molecules, with two being unexpectedly difficult cases for analysis with in-house diffractometers in regard to data quality and proper space-group determination. These issues were easily resolved by the use of synchrotron radiation using data-collectionmore » times of less than an hour. One of these guests induced a single-crystal-to-single-crystal transformation to create a larger unit cell with over 500 non-H atoms in the asymmetric unit. This led to a non-trivial refinement scenario that afforded the best Flack x absolute stereochemical determination parameter to date for these systems. The structures did not require the use of PLATON/SQUEEZE or other solvent-masking programs, and are the highest-quality crystalline sponge systems reported to date where the results are strongly supported by the data. A set of guidelines for the entire crystallographic process were developed through these studies. In particular, the refinement guidelines include strategies to refine the host framework, locate guests and determine occupancies, discussion of the proper use of geometric and anisotropic displacement parameter restraints and constraints, and whether to perform solvent squeezing/masking. The single-crystal-to-single-crystal transformation process for the crystal sponges is also discussed. The presented general guidelines will be invaluable for researchers interested in using the crystalline sponge method at in-house diffraction or synchrotron facilities, will facilitate the collection and analysis of reliable high-quality data, and will allow construction of chemically and physically sensible models for guest structural determination.« less

Non-covalent interactions in 2-methylimidazolium copper(II) complex (MeImH)2[Cu(pfbz)4]: Synthesis, characterization, single crystal X-ray structure and packing analysis

NASA Astrophysics Data System (ADS)

Sharma, Raj Pal; Saini, Anju; Kumar, Santosh; Kumar, Jitendra; Sathishkumar, Ranganathan; Venugopalan, Paloth

2017-01-01

A new anionic copper(II) complex, (MeImH)2 [Cu(pfbz)4] (1) where, MeImH = 2-methylimidazolium and pfbz = pentafluorobenzoate has been isolated by reacting copper(II) sulfate pentahydrate, pentafluorobenzoic acid and 2-methylimidazole in ethanol: water mixture in 1:2:2 molar ratio. This complex 1 has been characterized by elemental analysis, thermogravimetric analysis, spectroscopic techniques (UV-Vis, FT-IR) and conductance measurements. The complex salt crystallizes in monoclinic crystal system with space group C2/c. Single crystal X-ray structure determination revealed the presence of discrete ions: [Cu(pfbz)4]2- anion and two 2-methylimidazolium cation (C4H7N2)+. The crystal lattice is stabilized by strong hydrogen bonding and F⋯F interactions between cationic-anionic and the anionic-anionic moieties respectively, besides π-π interactions.

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

NASA Astrophysics Data System (ADS)

Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

2018-04-01

A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-Phenylalanine L-phenylalaninium malonate

NASA Astrophysics Data System (ADS)

Prakash, M.; Geetha, D.; Lydia Caroline, M.; Ramesh, P. S.

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric 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 180 °C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time.

van der Waals epitaxy of SnS film on single crystal graphene buffer layer on amorphous SiO2/Si

NASA Astrophysics Data System (ADS)

Xiang, Yu; Yang, Yunbo; Guo, Fawen; Sun, Xin; Lu, Zonghuan; Mohanty, Dibyajyoti; Bhat, Ishwara; Washington, Morris; Lu, Toh-Ming; Wang, Gwo-Ching

2018-03-01

Conventional hetero-epitaxial films are typically grown on lattice and symmetry matched single crystal substrates. We demonstrated the epitaxial growth of orthorhombic SnS film (∼500 nm thick) on single crystal, monolayer graphene that was transferred on the amorphous SiO2/Si substrate. Using X-ray pole figure analysis we examined the structure, quality and epitaxy relationship of the SnS film grown on the single crystal graphene and compared it with the SnS film grown on commercial polycrystalline graphene. We showed that the SnS films grown on both single crystal and polycrystalline graphene have two sets of orientation domains. However, the crystallinity and grain size of the SnS film improve when grown on the single crystal graphene. Reflection high-energy electron diffraction measurements show that the near surface texture has more phases as compared with that of the entire film. The surface texture of a film will influence the growth and quality of film grown on top of it as well as the interface formed. Our result offers an alternative approach to grow a hetero-epitaxial film on an amorphous substrate through a single crystal graphene buffer layer. This strategy of growing high quality epitaxial thin film has potential applications in optoelectronics.

Synthesis, characterization and single crystal x-ray analysis of a complex of iron(II) bis(2,4-dimethylphenyl)dithiophosphate with 4-ethylpyridine

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Sandeep; Andotra, Savit; Kaur, Mandeep

2016-09-15

Complex of iron(II) bis(2,4-dimethylphenyl)dithiophosphate with 4-ethylpyridine [((2,4- (CH{sub 3}){sub 2}C{sub 6}H{sub 3}O)2PS2)2Fe(NC{sub 5}H{sub 4}(C{sub 2}H{sub 5})-4){sub 2}] is synthesized and characterized by elemental analysis, magnetic moment, IR spectroscopy and single crystal X-ray analysis. Complex crystallizes in the monoclinic sp. gr. P2{sub 1}/n, Z = 2. Crystal structure consists of mononuclear units with Fe(II) ion chelated by four S atoms of the two diphenyldithiophosphate ligands in bidentate manner. N atoms from two 4-ethylpyridine ligands are axially coordinated to the Fe(II) atom leading to an octahedral geometry.

Crystal structure, Raman scattering and magnetic properties of CuCr2-xZrxSe4 and CuCr2-xSnxSe4 selenospinels

NASA Astrophysics Data System (ADS)

Pinto, C.; Galdámez, A.; Barahona, P.; Moris, S.; Peña, O.

2018-06-01

Selenospinels, CuCr2-xMxSe4 (M = Zr and Sn), were synthesized via conventional solid-state reactions. The crystal structure of CuCr1.5Sn0.5Se4, CuCr1.7Sn0.3Se4, CuCr1.5Zr0.5Se4, and CuCr1.8Zr0.2Se4 were determined using single-crystal X-ray diffraction. All the phases crystallized in a cubic spinel-type structure. The chemical compositions of the single-crystals were examined using energy-dispersive X-ray analysis (EDS). Powder X-ray diffraction patterns of CuCr1.3Sn0.7Se4 and CuCr1.7Sn0.3Se4 were consistent with phases belonging to the Fd 3 bar m Space group. An analysis of the vibrational properties on the single-crystals was performed using Raman scattering measurements. The magnetic properties showed a spin glass behavior with increasing Sn content and ferromagnetic order for CuCr1.7Sn0.3Se4.

Synthesis, growth and characterization of a nonlinear optical crystal: Bis l-proline hydrogen nitrate.

PubMed

Selvaraju, K; Kirubavathi, K

2013-11-01

The single crystals of bis l-proline hydrogen nitrate (BLPHN) belonging to non-centrosymmetric space group were successfully grown by the slow evaporation solution growth technique. The BLPHN crystals of size 10×7×3mm(3) were obtained in 35days. Initially, the solubility tests were carried out for two solvents such as deionized water and mixed of deionized water-acetone. Among the two solvents, the solubility of BLPHN was found to be the highest in deionized water, so crystallization of BLPHN was done from its aqueous solution. As grown, crystals were characterized by single crystal X-ray diffraction studies and optical transmission spectral studies. Infrared spectroscopy, thermo gravimetric analysis and differential thermal analysis measurements were performed to study the molecular vibration and thermal behavior of the grown BLPHN crystals. Nonlinear optical (NLO) behavior of BLPHN crystal was studied by Kurtz and Perry powder method. Copyright © 2013 Elsevier B.V. All rights reserved.

Constitutive Modeling of Superalloy Single Crystals and Directionally Solidified Materials

NASA Technical Reports Server (NTRS)

Walker, K. P.; Jordan, E. H.

1985-01-01

A unified viscoplastic constitutive relation based on crystallographic slip theory was developed for the deformation analysis of nickel base face centered cubic superalloy single crystals at elevated temperature. The single crystal theory is embedded in a self consistent method to derive a constitutive relation for a directionally solidified material comprised of a polycrystalline aggregate of columnar cylindrical grains. One of the crystallographic axes of the cylindrical crystals points in the columnar direction while the remaining crystallographic axes are oriented at random in the basal plane perpendicular to the columnar direction. These constitutive formulations are coded in FORTRAN for use in nonlinear finite element and boundary element programs.

Iron single crystal growth from a lithium-rich melt

NASA Astrophysics Data System (ADS)

Fix, M.; Schumann, H.; Jantz, S. G.; Breitner, F. A.; Leineweber, A.; Jesche, A.

2018-03-01

α -Fe single crystals of rhombic dodecahedral habit were grown from a Li84N12Fe∼3 melt. Crystals of several millimeter along a side form at temperatures around T ≈ 800 ° C. Upon further cooling the growth competes with the formation of Fe-doped Li3N. The b.c.c. structure and good sample quality of α -Fe single crystals were confirmed by X-ray and electron diffraction as well as magnetization measurements and chemical analysis. A nitrogen concentration of 90 ppm was detected by means of carrier gas hot extraction. Scanning electron microscopy did not reveal any sign of iron nitride precipitates.

RNi2B2C (R = Ho, Dy, Tb and Pr) single crystals grown by the cold copper crucible method

NASA Astrophysics Data System (ADS)

Durán, A.; Munoz, E.; Bernès, S.; Escudero, R.

2000-08-01

Single crystals of RNi2B2C (R = Ho, Dy, Tb, Pr) have been grown on cold copper crucibles in a high-frequency induction furnace. As a result, shiny metallic and brittle platelike single crystals were obtained. They were examined by x-ray and scanning electron microscopy with WDX/EDX for local composition analysis and show a very good crystallographic structure and compositions. Resistivity and dc magnetic measurements were performed to study superconducting and magnetic properties. Besides known electronic properties of the RNi2B2C family, we report for the first time results for PrNi2B2C single crystals successfully obtained by this technique.

Epitaxial Growth of an Organic p-n Heterojunction: C60 on Single-Crystal Pentacene.

PubMed

Nakayama, Yasuo; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Tsuruta, Ryohei; Hinderhofer, Alexander; Gerlach, Alexander; Broch, Katharina; Belova, Valentina; Frank, Heiko; Yamamoto, Masayuki; Niederhausen, Jens; Glowatzki, Hendrik; Rabe, Jürgen P; Koch, Norbert; Ishii, Hisao; Schreiber, Frank; Ueno, Nobuo

2016-06-01

Designing molecular p-n heterojunction structures, i.e., electron donor-acceptor contacts, is one of the central challenges for further development of organic electronic devices. In the present study, a well-defined p-n heterojunction of two representative molecular semiconductors, pentacene and C60, formed on the single-crystal surface of pentacene is precisely investigated in terms of its growth behavior and crystallographic structure. C60 assembles into a (111)-oriented face-centered-cubic crystal structure with a specific epitaxial orientation on the (001) surface of the pentacene single crystal. The present experimental findings provide molecular scale insights into the formation mechanisms of the organic p-n heterojunction through an accurate structural analysis of the single-crystalline molecular contact.

Studies on synthesis, growth, structural, thermal, linear and nonlinear optical properties of organic picolinium maleate single crystals.

PubMed

Pandi, P; Peramaiyan, G; Sudhahar, S; Chakkaravarthi, G; Mohan Kumar, R; Bhagavannarayana, G; Jayavel, R

2012-12-01

Picolinium maleate (PM), an organic material has been synthesised and single crystals were grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction analysis. PM crystal belongs to the monoclinic crystallographic system with space group P2(1)/c. The crystalline perfection of the grown crystals was analyzed by high-resolution X-ray diffraction rocking curve measurements. The presence of functional groups in PM was identified by FTIR and FT-NMR spectral analyses. Thermal behaviour and stability of picolinium maleate were studied by TGA/DTA analyses. UV-Vis spectral studies reveal that PM crystals are transparent in the wavelength region 327-1100 nm. The laser damage threshold value of PM crystal was found to be 4.3 GW/cm(2) using Nd:YAG laser. The Kurtz and Perry powder second harmonic generation technique confirms the nonlinear optical property of the grown crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

Enhanced optical, thermal and piezoelectric behavior in dye doped potassium acid phthalate (KAP) single crystal

NASA Astrophysics Data System (ADS)

Rao, G. Babu; Rajesh, P.; Ramasamy, P.

2017-06-01

Dye inclusion crystals have attracted researchers in the context of crystal growth for applications in solid state lasers. Pure and 0.1 mol% amaranth doped KAP single crystals, were grown from aqueous solutions by slow evaporation technique at room temperature. The grown crystals are up to the dimension of 12×10×3 mm3. Attempt is made to improve the growth rate, optical, piezoelectric and photoconductive properties of pure KAP single crystal with addition of amaranth dye as a dopant. Various characterization studies were made for both pure and dye doped KAP. Thermal stability of the crystals is tested from thermogravimetric and differential thermal analysis (TG/DTA). There is only one endothermic peak indicating decomposition point. Higher optical transparency for dye doped KAP crystal was identified from the UV-vis spectrum. Etching studies showed an improvement in the optical quality of the KAP crystal after doping with amaranth dye. The positive photoconductive nature is observed from both pure and amaranth doped KAP.

Design and analysis of large-core single-mode windmill single crystal sapphire optical fiber

DOE PAGES

Cheng, Yujie; Hill, Cary; Liu, Bo; ...

2016-06-01

We present a large-core single-mode “windmill” single crystal sapphire optical fiber (SCSF) design, which exhibits single-mode operation by stripping off the higher-order modes (HOMs) while maintaining the fundamental mode. The “windmill” SCSF design was analyzed using the finite element analysis method, in which all the HOMs are leaky. The numerical simulation results show single-mode operation in the spectral range from 0.4 to 2 μm in the windmill SCSF, with an effective core diameter as large as 14 μm. Such fiber is expected to improve the performance of many of the current sapphire fiber optic sensor structures.

Optical and dielectric studies of KH2PO4 crystal influenced by organic ligand of citric acid and L-valine: A single crystal growth and comparative study

NASA Astrophysics Data System (ADS)

Anis, Mohd; Hakeem, D. A.; Muley, G. G.

In the present study pure, citric acid (CA) and L-valine (LV) doped potassium dihydrogen phosphate (KDP) crystals have been grown with the aim to investigate the nonlinear optical applications facilitated by UV-visible, third order nonlinear optical (TONLO) and dielectric properties. The structural parameters of grown crystals have been confirmed by single crystal X-ray diffraction analysis. The enhancement in optical transparency of KDP crystal due to addition of CA and LV has been examined within 200-900 nm by means of UV-visible spectral analysis. In addition, the transmittance data have been used to evaluate the effect of dopants on reflectance, refractive index and extinction coefficient of grown crystals in the visible region. The Z-scan analysis has been performed at 632.8 nm to identify the nature of photoinduced nonlinear refraction and nonlinear absorption in doped KDP crystals. The influence of π-bonded ligand of dopant CA and LV on TONLO susceptibility (χ3), refractive index (n2) and absorption coefficient (β) of KDP crystals has been evaluated to discuss laser assisted device applications. The decrease in dielectric constant and dielectric loss of KDP crystal due to addition of CA and LV has been explored using the temperature dependent dielectric studies.

Growth, structural, optical, thermal and mechanical properties of ammonium pentaborate single crystal.

PubMed

Balakrishnan, T; Bhagavannarayana, G; Ramamurthi, K

2008-11-15

Nonlinear optical single crystals of ammonium pentaborate (APB) were grown by the slow cooling method from aqueous solution. Grown crystal was characterized by powder X-ray diffraction (PXRD) and FT-IR spectral analysis. Perfection of the grown crystal was evaluated by high-resolution X-ray diffractometry (HRXRD). The effect of nylon threading on the perfection of the grown bigger crystal was also studied by HRXRD. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties were investigated by TG-DTA and DSC analyses. Its mechanical hardness was estimated by Vickers microhardness tester.

On the morphological and chemical stability of vitamin C crystals

NASA Astrophysics Data System (ADS)

Halász, Susan; Bodor, Beáta

1993-03-01

Mass cooling crystallization of aqueous vitamin C solution was studied by applying different cooling rates, initial supersaturations and mixing intensity. The morphology of the products (size, habit and colour) well followed the changes of process parameters. Comparing a high purity (99.9%) standard with a yellow coloured heterodisperse product and a slowly grown single crystal, HPLC chromatography detected decreasing purity of the bigger single crystals, while X-ray and NMR analysis did not show any perceptible difference. It has been concluded that not the surface oxidation (chemical degredation), but rather the inclusions are the main sources of impurities within the crystals.

Phase transition in a multiferroic Ni-Mn-Ga single crystal

NASA Astrophysics Data System (ADS)

Veřtát, P.; Drahokoupil, J.; Perevertov, O.; Heczko, O.

2016-08-01

We studied martensitic phase transformation, crystal structure and twinned microstructure of resulting martensite of a Ni-Mn-Ga single crystal as essential conditions for magnetic shape memory effect. Thermal dependence of electric resistivity, magnetic susceptibility and dilatation measurements were measured to characterise kinetics of the transformation. With the help of XRD analysis and optical microscopy we evaluated the hierarchical twinning microstructure in the 10M martensite.

Single crystal growth and characterization of kagomé-lattice shandites Co3Sn2-xInxS2

NASA Astrophysics Data System (ADS)

Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

2015-09-01

Single crystals of the shandite-type half metallic ferromagnet Co3Sn2S2, and its In-substituted compounds, Co3Sn2-xInxS2 (0

Kinetic products in coordination networks: ab initio X-ray powder diffraction analysis.

PubMed

Martí-Rujas, Javier; Kawano, Masaki

2013-02-19

Porous coordination networks are materials that maintain their crystal structure as molecular "guests" enter and exit their pores. They are of great research interest with applications in areas such as catalysis, gas adsorption, proton conductivity, and drug release. As with zeolite preparation, the kinetic states in coordination network preparation play a crucial role in determining the final products. Controlling the kinetic state during self-assembly of coordination networks is a fundamental aspect of developing further functionalization of this class of materials. However, unlike for zeolites, there are few structural studies reporting the kinetic products made during self-assembly of coordination networks. Synthetic routes that produce the necessary selectivity are complex. The structural knowledge obtained from X-ray crystallography has been crucial for developing rational strategies for design of organic-inorganic hybrid networks. However, despite the explosive progress in the solid-state study of coordination networks during the last 15 years, researchers still do not understand many chemical reaction processes because of the difficulties in growing single crystals suitable for X-ray diffraction: Fast precipitation can lead to kinetic (metastable) products, but in microcrystalline form, unsuitable for single crystal X-ray analysis. X-ray powder diffraction (XRPD) routinely is used to check phase purity, crystallinity, and to monitor the stability of frameworks upon guest removal/inclusion under various conditions, but rarely is used for structure elucidation. Recent advances in structure determination of microcrystalline solids from ab initio XRPD have allowed three-dimensional structure determination when single crystals are not available. Thus, ab initio XRPD structure determination is becoming a powerful method for structure determination of microcrystalline solids, including porous coordination networks. Because of the great interest across scientific disciplines in coordination networks, especially porous coordination networks, the ability to determine crystal structures when the crystals are not suitable for single crystal X-ray analysis is of paramount importance. In this Account, we report the potential of kinetic control to synthesize new coordination networks and we describe ab initio XRPD structure determination to characterize these networks' crystal structures. We describe our recent work on selective instant synthesis to yield kinetically controlled porous coordination networks. We demonstrate that instant synthesis can selectively produce metastable networks that are not possible to synthesize by conventional solution chemistry. Using kinetic products, we provide mechanistic insights into thermally induced (573-723 K) (i.e., annealing method) structural transformations in porous coordination networks as well as examples of guest exchange/inclusion reactions. Finally, we describe a memory effect that allows the transfer of structural information from kinetic precursor structures to thermally stable structures through amorphous intermediate phases. We believe that ab initio XRPD structure determination will soon be used to investigate chemical processes that lead intrinsically to microcrystalline solids, which up to now have not been fully understood due to the unavailability of single crystals. For example, only recently have researchers used single-crystal X-ray diffraction to elucidate crystal-to-crystal chemical reactions taking place in the crystalline scaffold of coordination networks. The potential of ab initio X-ray powder diffraction analysis goes beyond single-crystal-to-single-crystal processes, potentially allowing members of this field to study intriguing in situ reactions, such as reactions within pores.

Synthesis and structural characterization of bulk Sb2Te3 single crystal

NASA Astrophysics Data System (ADS)

Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

2018-05-01

We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

Insertion of Guest Molecules into a Mixed Ligand Metal-Organic Framework via Single-Crystal-to-Single Crystal Guest Exchange

DTIC Science & Technology

2014-07-01

powder x-ray diffraction (PXRD), thermogravimentric analysis (TGA), and Fourier transform infrared (FTIR). 15. SUBJECT TERMS Metal organic frame work...the inclusion by using a variety of analytical techniques, such as powder x-ray diffraction (PXRD), thermo-gravimetric analysis (TGA), Fourier...Characterizations Analysis of the MOF and the complexes with the MOF and the guest molecules was performed using an Agilent GC-MS (Model 6890N GC and Model 5973N

Antimicrobial activity and second harmonic studies on organic non-centrosymmetric pure and doped ninhydrin single crystals

NASA Astrophysics Data System (ADS)

Prasanyaa, T.; Jayaramakrishnan, V.; Haris, M.

2013-03-01

In this paper, we report the successful growth of pure, Cu2+ ions and Cd2+ ions doped on ninhydrin single crystals by slow solvent evaporation technique. The presence of Cu2+ and Cd2+ ions in the specimen of ninhydrin single crystal has been determined by atomic absorption spectroscopy. The powder X-ray diffraction analysis was done to calculate the lattice parameters of the pure and doped crystals. The percentage of transmittance of the crystal was recorded using the UV-Vis Spectrophotometer. Thermal behaviors of the grown crystals have been examined by the thermal gravimetric/differential thermal analysis. The hardness of the grown crystals was assessed and the results show the minor variation in the hardness value for the pure and doped ninhydrin samples. The value of the work hardening coefficient n was found to be 2.0, 1.0 and 1.06 for pure, copper and cadmium doped ninhydrin crystals respectively. The second harmonic generation efficiency of Cd2+ and Cu2+ doped ninhydrin is 8.3 and 6.3 times greater than well known nonlinear crystal of potassium dihydrogen phosphate respectively. The antibacterial and antifungal activities of the title compound were performed by disk diffusion method against the standard bacteria Escherichia coli, Xanthomonas oryzae and against the fungus Aspergillis niger and Aspergillus flavus.

Growth and characterization of an organic single crystal: 2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide

NASA Astrophysics Data System (ADS)

Senthil, K.; Kalainathan, S.; Ruban Kumar, A.

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. 1H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker’s hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal.

Antimicrobial activity and second harmonic studies on organic non-centrosymmetric pure and doped ninhydrin single crystals.

PubMed

Prasanyaa, T; Jayaramakrishnan, V; Haris, M

2013-03-01

In this paper, we report the successful growth of pure, Cu(2+) ions and Cd(2+) ions doped on ninhydrin single crystals by slow solvent evaporation technique. The presence of Cu(2+) and Cd(2+) ions in the specimen of ninhydrin single crystal has been determined by atomic absorption spectroscopy. The powder X-ray diffraction analysis was done to calculate the lattice parameters of the pure and doped crystals. The percentage of transmittance of the crystal was recorded using the UV-Vis Spectrophotometer. Thermal behaviors of the grown crystals have been examined by the thermal gravimetric/differential thermal analysis. The hardness of the grown crystals was assessed and the results show the minor variation in the hardness value for the pure and doped ninhydrin samples. The value of the work hardening coefficient n was found to be 2.0, 1.0 and 1.06 for pure, copper and cadmium doped ninhydrin crystals respectively. The second harmonic generation efficiency of Cd(2+) and Cu(2+) doped ninhydrin is 8.3 and 6.3 times greater than well known nonlinear crystal of potassium dihydrogen phosphate respectively. The antibacterial and antifungal activities of the title compound were performed by disk diffusion method against the standard bacteria Escherichia coli, Xanthomonas oryzae and against the fungus Aspergillis niger and Aspergillus flavus. Copyright © 2012 Elsevier B.V. All rights reserved.

Studies on the synthesis, spectral, optical and thermal properties of l-Valine Zinc Sulphate: an organic inorganic hybrid nonlinear optical crystal.

PubMed

Puhal Raj, A; Ramachandra Raja, C

2012-11-01

Nonlinear optical (NLO) organic inorganic hybrid l-Valine Zinc Sulphate (LVZS) was synthesized and single crystals were obtained from saturated aqueous solution by slow evaporation method at 36°C using a constant temperature bath (CTB) with an accuracy of ±0.01°C. This crystal is reported with its characterization by single crystal and powder XRD, FTIR, UV-Vis-NIR, TG/DTA analysis and SHG test. Single crystal XRD study reveals that LVZS crystallizes in monoclinic system with the lattice constants a=9.969(3) Å, b=7.238(3) Å, c=24.334(9) Å and cell volume is 1736.00Å(3). Sharp peaks observed in powder X-ray diffraction studies confirm the high degree of crystallinity of grown crystal. The incorporation of sulphate ion with l-valine is confirmed by FTIR spectrum in LVZS crystal(.) A remarkable increase in optical transparency has been observed in LVZS when compared to l-valine and zinc sulphate heptahydrate Thermal properties of LVZS have been reported by using TG/DTA analysis. Kurtz powder second harmonic generation (SHG) test confirms NLO property of the crystal and SHG efficiency of LVZS was found to be 1.34 times more than pure l-valine. Copyright © 2012 Elsevier B.V. All rights reserved.

Experimental and density functional theory (DFT): A dual approach to probe the key properties of creatininium L-tartrate monohydrate single crystal for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Thirumurugan, R.; Babu, B.; Anitha, K.; Chandrasekaran, J.

2017-12-01

A novel organic nonlinear optical (NLO) material, creatininium L-tartrate monohydrate (CTM) was synthesized and it was grown as single crystals with optical quality. 1H and 13C NMR spectral studies were performed and molecular structure of synthesized CTM compound was confirmed. Single crystal X-ray diffraction (SXRD) analysis confirmed that CTM was crystallized in orthorhombic system with non-centrosymmetric (NCS), P212121, space group. The grown crystal exhibited admirable properties such as second harmonic generation efficiency (SHG) (1.9 times KDP), and high laser damage threshold (LDT) value of 3.7 GW cm-2. CTM crystal displayed high transparency (∼60%) in the visible and near-IR region with low cut-off wavelength at 249 nm. Photoluminescence study confirmed blue wavelength emission (∼463 nm) of grown crystal. Thermal and mechanical behaviours have been successfully analysed for grown crystals. The dielectric studies were carried out for grown crystal as a function of frequencies at different temperatures. Hirshfeld surface and fingerprint plots provided the percentage of individual interactions contributed by each atom. Moreover, density functional theory (DFT) calculations have been employed to probe the frontier molecular orbitals (FMOs) and first hyperpolarizability (β) analysis of the optimized CTM structure. These results validated CTM as a suitable NLO candidate and were discussed in this work.

Growth and characterization of an organic single crystal: 2-[2-(4-diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide.

PubMed

Senthil, K; Kalainathan, S; Ruban Kumar, A

2014-05-05

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. (1)H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker's hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prokhorov, I. A., E-mail: igor.prokhorov@mail.ru; Ralchenko, V. G.; Bolshakov, A. P.

2013-12-15

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likelymore » due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.« less

Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

NASA Astrophysics Data System (ADS)

Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

2017-06-01

The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.

Morphological, spectroscopic and thermal studies of samarium chloride coordinated single crystal grown by slow evaporation method

NASA Astrophysics Data System (ADS)

Slathia, Goldy; Raina, Bindu; Gupta, Rashmi; Bamzai, K. K.

2018-05-01

The synthesis of samarium chloride coordinated single crystal was carried out at room temperature by slow evaporation method. The crystal possesses a well defined hexagonal morphology with six symmetrically equivalent growth sectors separated by growth boundaries. The theoretical morphology has been established by structural approach using Bravaise-Friedele-Donnaye-Harker (BFDH) law. Fourier transform infra red spectroscopy was carried in order to study the geometry and structure of the crystal. The detailed thermogravimetric analysis elucidates the thermal stability of the complex.

Growth, spectral and optical characterization of a novel nonlinear optical organic material: D-Alanine DL-Mandelic acid single crystal

NASA Astrophysics Data System (ADS)

Jayaprakash, P.; Mohamed, M. Peer; Caroline, M. Lydia

2017-04-01

An organic nonlinear optical single crystal, D-alanine DL-mandelic acid was synthesized and successfully grown by slow evaporation solution growth technique at ambient temperature using solvent of aqueous solution. The unit cell parameters were assessed from single crystal X-ray diffraction analysis. The presence of diverse functional groups and vibrational modes were identified using Fourier Transform Infra Red and Fourier Transform Raman spectral analyses. The chemical structure of grown crystal has been identified by Nuclear Magnetic Resonance spectroscopic study. Ultraviolet-visible spectral analysis reveal that the crystal has lower cut-off wavelength down to 259 nm, is a key factor to exhibit second harmonic generation signal. The electronic optical band gap and Urbach energy is calculated as 5.31 eV and 0.2425 eV respectively from the UV absorption profile. The diverse optical properties such as, extinction coefficient, reflectance, linear refractive index, optical conductivity was calculated using UV-visible data. The relative second harmonic efficiency of the compound is found to be 0.81 times greater than that of KH2PO4 (KDP). The thermal stability of the grown crystal was studied by thermogravimetric analysis and differential thermal analysis techniques. The luminescence spectrum exhibited two peaks (520 nm, 564 nm) due to the donation of protons from carboxylic acid to amino group. The Vickers microhardness test was carried out employing one of the as-grown hard crystal and there by hardness number (Hv), Meyer's index (n), yield strength (σy), elastic stiffness constant (C11) and Knoop hardness number (HK) were assessed. The dielectric behaviour of the as-grown crystal was analyzed for different temperatures (313 K, 333 K, 353 K, and 373 K) at different frequencies.

Multiphysical simulation analysis of the dislocation structure in germanium single crystals

NASA Astrophysics Data System (ADS)

Podkopaev, O. I.; Artemyev, V. V.; Smirnov, A. D.; Mamedov, V. M.; Sid'ko, A. P.; Kalaev, V. V.; Kravtsova, E. D.; Shimanskii, A. F.

2016-09-01

To grow high-quality germanium crystals is one of the most important problems of growth industry. The dislocation density is an important parameter of the quality of single crystals. The dislocation densities in germanium crystals 100 mm in diameter, which have various shapes of the side surface and are grown by the Czochralski technique, are experimentally measured. The crystal growth is numerically simulated using heat-transfer and hydrodynamics models and the Alexander-Haasen dislocation model in terms of the CGSim software package. A comparison of the experimental and calculated dislocation densities shows that the dislocation model can be applied to study lattice defects in germanium crystals and to improve their quality.

Synthesis, crystal growth, optical, thermal, and mechanical properties of a nonlinear optical single crystal: ammonium sulfate hydrogen sulphamate (ASHS)

NASA Astrophysics Data System (ADS)

Sudhakar, K.; Nandhini, S.; Muniyappan, S.; Arumanayagam, T.; Vivek, P.; Murugakoothan, P.

2018-04-01

Ammonium sulfate hydrogen sulphamate (ASHS), an inorganic nonlinear optical crystal, was grown from the aqueous solution by slow evaporation solution growth technique. The single-crystal XRD confirms that the grown single crystal belongs to the orthorhombic system with the space group of Pna21. Powder XRD confirms the crystalline nature and the diffraction planes were indexed. Crystalline perfection of grown crystal was analysed by high-resolution X-ray diffraction rocking curve technique. UV-Vis-NIR studies revealed that ASHS crystal has optical transparency 65% and lower cut-off wavelength at 218 nm. The violet light emission of the crystal was identified by photoluminescence studies. The particle size-dependent second-harmonic generation efficiency for ASHS crystal was evaluated by Kurtz-Perry powder technique using Nd:YAG laser which established the existence of phase matching. Surface laser damage threshold value was evaluated using Nd:YAG laser. Optical homogeneity of the crystal was evaluated using modified channel spectrum method through birefringence study. Thermal analysis reveals that ASHS crystal is stable up to 213 °C. The mechanical behaviour of the ASHS crystal was analysed using Vickers microhardness study.

Studies on the growth aspects, structural, thermal, dielectric and third order nonlinear optical properties of solution grown 4-methylpyridinium p-nitrophenolate single crystal

NASA Astrophysics Data System (ADS)

Devi, S. Reena; Kalaiyarasi, S.; Zahid, I. MD.; Kumar, R. Mohan

2016-11-01

An ionic organic optical crystal of 4-methylpyridinium p-nitrophenolate was grown from methanol by slow evaporation method at ambient temperature. Powder and single crystal X-ray diffraction studies revealed the crystal system and its crystalline perfection. The rocking curve recorded from HRXRD study confirmed the crystal quality. FTIR spectral analysis confirmed the functional groups present in the title compound. UV-visible spectral study revealed the optical window and band gap of grown crystal. The thermal, electrical and surface laser damage threshold properties of harvested crystal were examined by using TGA/DTA, LCR/Impedance Analyzer and Nd:YAG laser system respectively. The third order nonlinear optical property of grown crystal was elucidated by Z-scan technique.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ramadhar, Timothy R.; Zheng, Shao -Liang; Chen, Yu -Sheng

A detailed set of synthetic and crystallographic guidelines for the crystalline sponge method based upon the analysis of expediently synthesized crystal sponges using third-generation synchrotron radiation are reported. The procedure for the synthesis of the zinc-based metal–organic framework used in initial crystal sponge reports has been modified to yield competent crystals in 3 days instead of 2 weeks. These crystal sponges were tested on some small molecules, with two being unexpectedly difficult cases for analysis with in-house diffractometers in regard to data quality and proper space-group determination. These issues were easily resolved by the use of synchrotron radiation using data-collectionmore » times of less than an hour. One of these guests induced a single-crystal-to-single-crystal transformation to create a larger unit cell with over 500 non-H atoms in the asymmetric unit. This led to a non-trivial refinement scenario that afforded the best Flack x absolute stereochemical determination parameter to date for these systems. The structures did not require the use of PLATON/SQUEEZE or other solvent-masking programs, and are the highest-quality crystalline sponge systems reported to date where the results are strongly supported by the data. A set of guidelines for the entire crystallographic process were developed through these studies. In particular, the refinement guidelines include strategies to refine the host framework, locate guests and determine occupancies, discussion of the proper use of geometric and anisotropic displacement parameter restraints and constraints, and whether to perform solvent squeezing/masking. The single-crystal-to-single-crystal transformation process for the crystal sponges is also discussed. The presented general guidelines will be invaluable for researchers interested in using the crystalline sponge method at in-house diffraction or synchrotron facilities, will facilitate the collection and analysis of reliable high-quality data, and will allow construction of chemically and physically sensible models for guest structural determination.« less

Crystal growth, structural, optical, dielectric and thermal studies of an amino acid based organic NLO material: L-phenylalanine L-phenylalaninium malonate.

PubMed

Prakash, M; Geetha, D; Caroline, M Lydia; Ramesh, P S

2011-12-01

Good transparent single crystals of L-phenylalanine L-phenylalaninium malonate (LPPMA) have been grown successfully by slow evaporation technique from aqueous solution. Single crystal X-ray diffractometer was utilized to measure unit cell parameter and to confirm the crystal structure. The chemical structure of compound was established by FT-NMR technique. The vibrational modes of the molecules of elucidated from FTIR spectra. Its optical behaviour has been examined by UV-vis spectral analysis, which shows the absence of absorbance in the visible region. Thermal properties of the LPPMA crystal were carried out by thermo gravimetric 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 180°C by melting point apparatus. The NLO property was confirmed by the powder technique of Kurtz and Perry. The dielectric behaviour of the sample was also studied for the first time. Copyright © 2011 Elsevier B.V. All rights reserved.

Investigation on the growth, spectral, lifetime, mechanical analysis and third-order nonlinear optical studies of L-methionine admixtured D-mandelic acid single crystal: A promising material for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Jayaprakash, P.; Sangeetha, P.; Kumari, C. Rathika Thaya; Caroline, M. Lydia

2017-08-01

A nonlinear optical bulk single crystal of L-methionine admixtured D-mandelic acid (LMDMA) has been grown by slow solvent evaporation technique using water as solvent at ambient temperature. The crystallized LMDMA single crystal subjected to single crystal X-ray diffraction study confirmed monoclinic system with the acentric space group P21. The FTIR analysis gives information about the modes of vibration in the various functional groups present in LMDMA. The UV-visible spectral analysis assessed the optical quality and linear optical properties such as extinction coefficient, reflectance, refractive index and from which optical conductivity and electric susceptibility were also evaluated. The frequency doubling efficiency was observed using Kurtz Perry powder technique. A multiple shot laser was utilized to evaluate the laser damage threshold energy of the crystal. Discrete thermodynamic properties were carried out by TG-DTA studies. The hardness, Meyer's index, yield strength, elastic stiffness constant, Knoop hardness, fracture toughness and brittleness index were analyzed using Vickers microhardness tester. Layer growth pattern and the surface defect were examined by chemical etching studies using optical microscope. Fluorescence emission spectrum was recorded and lifetime was also studied. The electric field response of crystal was investigated from the dielectric studies at various temperatures at different frequencies. The third-order nonlinear optical response in LMDMA has been investigated using Z-scan technique with He-Ne laser at 632.8 nm and nonlinear parameters such as refractive index (n2), absorption coefficient (β) and susceptibility (χ3) investigated extensively for they are in optical phase conjucation, high-speed optical switches and optical dielectric devices.

Synthesis, structural, optical and thermal studies of an organic nonlinear optical 4-aminopyridinium maleate single crystal.

PubMed

Pandi, P; Peramaiyan, G; Kumar, M Krishna; Kumar, R Mohan; Jayavel, R

2012-03-01

Synthesis and growth of a novel organic nonlinear optical (NLO) crystal of 4-aminopyridinium maleate (4APM) in larger size by the slow evaporation solution growth technique are reported. Single crystal and powder X-ray diffraction analyses reveal that 4APM crystallizes in monoclinic system with space group P2(1) with cell parameters a=8.140(4)Å, b=5.457(5)Å, c=10.926(10)Å and volume=481.4(7)Å(3). The grown crystal has been characterized by Fourier transform infrared and UV-visible spectral analyses. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) have been carried out to study its thermal properties. Dielectric measurements have been carried out to study the distribution of charges within the crystal. The mechanical strength of the crystal has been studied by using Vickers' microhardness test. The etching studies have been carried out on the grown crystal. The Kurtz and Perry powder SHG technique confirms the NLO property of the grown crystal and the SHG efficiency of 4APM was found to be 4.8 times greater than that of KDP crystal. Copyright © 2011 Elsevier B.V. All rights reserved.

Increasing dissolution of trospium chloride by co-crystallization with urea

NASA Astrophysics Data System (ADS)

Skořepová, Eliška; Hušák, Michal; Čejka, Jan; Zámostný, Petr; Kratochvíl, Bohumil

2014-08-01

The search for various solid forms of an active pharmaceutical ingredient (API) is an important step in drug development. Our aim was to prepare co-crystals of trospium chloride, an anticholinergic drug used for the treatment of incontinence, and to investigate if they have advantageous properties for drug formulation. Phase identification was done by powder X-ray diffraction and single-crystal X-ray diffraction. The chemical composition was verified by solution NMR and the dissolution rate of the prepared phases was studied by IDR (intrinsic dissolution rate). For further analysis of phase stability and transitions, combined thermal analysis and temperature-resolved X-ray powder diffraction were used. Urea was selected as a co-crystallization partner. Trospium chloride urea (1:1) co-crystal was prepared by a solvent evaporation. From single-crystal data, the co-crystal structure was solved in a space group P21/c and compared to previously published structures of trospium chloride. Intrinsic dissolution rate revealed that the co-crystal dissolves 32% faster than pure API. However, its low thermal and pressure stability makes it a challenging choice for the final drug formulation.

Experimental and numerical analysis of penetration/removal response of endodontic instrument made of single crystal Cu-based SMA: comparison with NiTi SMA instruments

NASA Astrophysics Data System (ADS)

Vincent, M.; Xolin, P.; Gevrey, A.-M.; Thiebaud, F.; Engels-Deutsch, M.; Ben Zineb, T.

2017-04-01

This paper presents an experimental and numerical study showing that single crystal shape memory alloy (SMA) Cu-based endodontic instruments can lead to equivalent mechanical performances compared to NiTi-based instruments besides their interesting biological properties. Following a previous finite element analysis (FEA) of single crystal CuAlBe endodontic instruments (Vincent et al 2015 J. Mater. Eng. Perform. 24 4128-39), prototypes with the determined geometrical parameters were machined and experimentally characterized in continuous rotation during a penetration/removal (P/R) protocol in artificial canals. The obtained mechanical responses were compared to responses of NiTi endodontic files in the same conditions. In addition, FEA was conducted and compared with the experimental results to validate the adopted modeling and to evaluate the local quantities inside the instrument as the stress state and the distribution of volume fraction of martensite. The obtained results highlight that single crystal CuAlBe SMA prototypes show equivalent mechanical responses to its NiTi homologous prototypes in the same P/R experimental conditions.

Experimental and computational studies on creatininium 4-nitrobenzoate - An organic proton transfer complex

NASA Astrophysics Data System (ADS)

Thirumurugan, R.; Anitha, K.

2017-10-01

A new organic proton transfer complex of creatininium 4-nitrobenzoate (C4NB) has been synthesized and its single crystals were grown successfully by slow evaporation technique. The grown single crystal was subjected to various characterization techniques like single crystal X-ray diffraction (SCXRD), FTIR, FT-Raman and Kurtz-Perry powder second harmonic generation (SHG). The SCXRD analysis revealed that C4NB was crystallized into orthorhombic crystal system, with noncentrosymmetric (NCS), P212121 space group. The creatininium cation and 4-nitrobenzoate anion were connected through a pair of N__H⋯O hydrogen bonds (N(3)__H(6) ⋯ O(3) (x+1, y, z) and N(2)__H(5) &ctdot O(2) (x-1/2, -y-1/2, -z+2)) and fashioned a R22(8) ring motif. The crystal structure was stabilized by strong N__H⋯O and weak C__H⋯O intermolecular interactions and it was quantitatively analysed by Hirshfeld surface and fingerprint (FP) analysis. FTIR and FT-Raman studies confirmed the vibrational modes of functional groups present in C4NB compound indubitably. SHG efficiency of grown crystal was 4.6 times greater than that of standard potassium dihydrogen phosphate (KDP) material. Moreover, density functional theory (DFT) studies such as Mulliken charge distribution, frontier molecular orbitals (FMOs), molecular electrostatic potential (MEP) map, natural bond orbital analysis (NBO) and first order hyperpolarizability (β0) were calculated to explore the structure-property relationship.

Investigations on nucleation, HRXRD, optical, piezoelectric, polarizability and Z-scan analysis of L-arginine maleate dihydrate single crystals

NASA Astrophysics Data System (ADS)

Sakthy Priya, S.; Alexandar, A.; Surendran, P.; Lakshmanan, A.; Rameshkumar, P.; Sagayaraj, P.

2017-04-01

An efficient organic nonlinear optical single crystal of L-arginine maleate dihydrate (LAMD) has been grown by slow evaporation solution technique (SEST) and slow cooling technique (SCT). The crystalline perfection of the crystal was examined using high-resolution X-ray diffractometry (HRXRD) analysis. Photoluminescence study confirmed the optical properties and defects level in the crystal lattice. Electromechanical behaviour was observed using piezoelectric co-efficient (d33) analysis. The photoconductivity analysis confirmed the negative photoconducting nature of the material. The dielectric constant and loss were measured as a function of frequency with varying temperature and vice-versa. The laser damage threshold (LDT) measurement was carried out using Nd:YAG Laser with a wavelength of 1064 nm (Focal length is 35 cm) and the obtained results showed that LDT value of the crystal is high compared to KDP crystal. The high laser damage threshold of the grown crystal makes it a potential candidate for second and higher order nonlinear optical device application. The third order nonlinear optical parameters of LAMD crystal is determined by open-aperture and closed-aperture studies using Z-scan technique. The third order linear and nonlinear optical parameters such as the nonlinear refractive index (n2), two photon absorption coefficient (β), Real part (Reχ3) and imaginary part (Imχ3) of third-order nonlinear optical susceptibility are calculated.

Crystallization, Crystal Orientation and Morphology of Poly(ethylene oxide) under 1D Defect-Free Nanoscale Confinement

NASA Astrophysics Data System (ADS)

Hsiao, Ming-Siao; Zheng, Joseph X.; van Horn, Ryan M.; Quirk, Roderic P.; Thomas, Edwin L.; Lotz, Bernard; Cheng, Stephen Z. D.

2009-03-01

One-dimensional (1-D) defect-free nanoscale confinement is created by growing single crystals of PS-b-PEO block copolymers in dilute solution. Those defect-free, 1-D confined lamellae having different PEO layer thicknesses in PS-b-PEO lamellar single crystals (or crystal mats) were used to study the polymer recrystallization and crystal orientation evolution as a function of recrystallization temperature (Trx) because the Tg^PS is larger than Tm^PEO in the PS-b-PEO single crystal. The results are summarized as follows. First, by the combination of electron diffraction and known PEO crystallography, the crystallization of PEO only takes place at Trx<-5^oC. Meanwhile a unique tilted PEO orientation is formed at Trx >-5^oC after self-seeding. The origin of the formation of tilted chains in the PEO crystal will be addressed. Second, from the analysis of 2D WAXD patterns of crystal mats, it is shown that the change in PEO c-axis orientation from homogeneous at low Trx to homeotropic at higher Trx transitions sharply, within 1^oC. The mechanism inducing this dramatic change in crystal orientation will be investigated in detail.

Nonlinear optical and microscopic analysis of Cu2+ doped zinc thiourea chloride (ZTC) monocrystal

NASA Astrophysics Data System (ADS)

Ramteke, S. P.; Anis, Mohd; Pandian, M. S.; Kalainathan, S.; Baig, M. I.; Ramasamy, P.; Muley, G. G.

2018-02-01

Organometallic crystals offer considerable nonlinear response therefore, present article focuses on bulk growth and investigation of Cu2+ ion doped zinc thiourea chloride (ZTC) crystal to explore its technological impetus for laser assisted nonlinear optical (NLO) device applications. The Cu2+ ion doped ZTC bulk single crystal of dimension 03 × 2.4 × 0.4 cm3 has been grown from pH controlled aqueous solution by employing slow solvent evaporation technique. The structural analysis has been performed by means of single crystal X-ray diffraction technique. The doping of Cu2+ ion in ZTC crystal matrix has been confirmed by means of energy dispersive spectroscopic (EDS) technique. The origin of nonlinear optical properties in Cu2+ ion doped ZTC crystal has been studied by employing the Kurtz-Perry test and Z-scan analysis. The remarkable enhancement in second harmonic generation (SHG) efficiency of Cu2+ ion doped ZTC crystal with reference to ZTC crystal has been determined. The He-Ne laser assisted Z-scan analysis has been performed to determine the third order nonlinear optical (TONLO) nature of grown crystal. The TONLO parameters such as susceptibility, absorption coefficient, refractive index and figure of merit of Cu-ZTC crystal have been evaluated using the Z-scan transmittance data. The laser damage threshold of grown crystal to high intensity of Nd:YAG laser is found to be 706.2 MW/cm2. The hardness number, work hardening index, yield strength and elastic stiffness coefficient of grown crystal has been investigated under microhardness study. The etching study has been carried out to determine the growth likelihood, nature of etch pits and surface quality of grown crystal.

Influence of Oxidation in Starting Material Sn on Electric Transport Properties of SnSe Single Crystals

NASA Astrophysics Data System (ADS)

Yamashita, Aichi; Ogiso, Osamu; Matsumoto, Ryo; Tanaka, Masashi; Hara, Hiroshi; Tanaka, Hiromi; Takeya, Hiroyuki; Lee, Chul-Ho; Takano, Yoshihiko

2018-06-01

We found that the electronic transport property of SnSe single crystals was sensitively affected by oxidation in raw Sn. Semiconducting SnSe single crystals were obtained by using Sn of grain form as a starting material while powder Sn resulted in metallic SnSe. X-ray photoelectron spectroscopy analysis revealed that the surfaces of raw Sn were oxidized, which volume fraction is lower in grain Sn. This indicates that the amount of oxygen in raw Sn is the key factor for the electronic transport property of SnSe.

A novel structure of gel grown strontium cyanurate crystal and its structural, optical, electrical characterization

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Gopakumar, N.; Babu, K. Rajendra

2017-12-01

Strontium cyanurate crystals with novel structure and unique optical property like mechanoluminescence have been grown by conventional gel method. Transparent crystals were obtained. The single crystal X-ray diffraction analysis reveals the exquisite structure of the grown crystal. The crystal is centrosymmetric and has a three dimensional polymeric structure. The powder X ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal were identified by Fourier transform infrared spectroscopy. Elemental analysis confirmed the composition of the complex. A study of thermal properties was done by thermo gravimetric analysis and differential thermal analysis. The optical properties like band gap, refractive index and extinction coefficient were evaluated from the UV visible spectral analysis. The etching study was done to reveal the dislocations in the crystal which in turn explains mechanoluminescence emission. The mechanoluminescence property exhibited by the crystal makes it suitable for stress sensing applications. Besides being a centrosymmetric crystal, it also exhibits NLO behavior. Dielectric properties were studied and theoretical calculations of Fermi energy, valence electron plasma energy, penn gap and polarisability have been done.

Growth and characterization of metal halide perovskite crystals: Benzyltributyl ammonium tetrachloro manganate(II) monohydrate

NASA Astrophysics Data System (ADS)

Dhandapani, M.; Sugandhi, K.; Nithya, S.; Muthuraja, P.; Balachandar, S.; Aranganayagam, K. R.

2018-05-01

The perovskite type organic-inorganic hybrid benzyltributyl ammoniumtetrachloro manganate (II) monohydrates (BTBA-Mn) are synthesized and the single crystals are grown by slow evaporation solution growth technique. The structure of the grown crystals are confirmed by using X-ray diffraction (XRD), unit cell parameter analysis, Fourier transform Infrared (FTIR), elemental analysis and 13C-NMR spectral studies. Thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning colorimetric (DSC) analysis were carried out to understand thermal stability and occurrence of phase transition.

Growth, structural, optical, thermal and laser damage threshold studies of an organic single crystal: 1,3,5 – triphenylbenzene (TPB)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raja, R. Subramaniyan; Babu, G. Anandha; Ramasamy, P., E-mail: E-mail-ramasamyp@ssn.edu.in

2016-05-23

Good quality single crystals of pure hydrocarbon 1,3,5-Triphenylbenzene (TPB) have been successfully grown using toluene as a solvent using controlled slow cooling solution growth technique. TPB crystallizes in orthorhombic structure with the space group Pna2{sub 1}. The structural perfection of the grown crystal has been analysed by high resolution X-ray diffraction measurements. The range and percentage of the optical transmission are ascertained by recording the UV-vis spectrum. Thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) were used to study its thermal properties. Powder second harmonic generation studies were carried out to explore its NLO properties. Laser damage threshold valuemore » has been determined using Nd:YAG laser operating at 1064 nm.« less

Hirshfeld surface analyses and crystal structures of supramolecular self-assembly thiourea derivatives directed by non-covalent interactions

NASA Astrophysics Data System (ADS)

Gumus, Ilkay; Solmaz, Ummuhan; Binzet, Gun; Keskin, Ebru; Arslan, Birdal; Arslan, Hakan

2018-04-01

The novel N-(bis(3,5-dimethoxybenzyl)carbamothioyl)-4-R-benzamide (R: H, Cl, CH3 and OCH3) compounds have been synthesized and characterized by FT-IR, 1H NMR and 13C NMR spectroscopy. Their crystal structures were also determined by single-crystal X-ray diffraction studies. Hirshfeld surfaces analysis and their associated two dimensional fingerprint plots of compounds were used as theoretical approach to assess driving force for crystal structure formation via the intermolecular interactions in the crystal lattices of synthesized compounds. The study of X-ray single crystal diffraction and Hirshfeld surfaces analysis of the prepared compounds shows that hydrogen bonding and other weaker interactions such as Nsbnd H⋯S, weak Csbnd H⋯S, Csbnd H⋯O, Csbnd H⋯N and Csbnd H···π intermolecular interactions and π-π stacking, among molecules of synthesized compounds participate in a cooperative way to stabilize the supramolecular structures.

Zr 2Ir 6B with an eightfold superstructure of the cubic perovskite-like boride ZrIr 3B 0.5: Synthesis, crystal structure and bonding analysis

NASA Astrophysics Data System (ADS)

Hermus, Martin; Fokwa, Boniface P. T.

2010-04-01

Single phase powder samples and single crystals of Zr 2Ir 6B were successfully synthesized by arc-melting the elements in a water-cooled copper crucible under an argon atmosphere. Superstructure reflections were observed both on powder and on single crystal diffraction data, leading to an eightfold superstructure of ZrIr 3B x phase. The new phase, which has a metallic luster, crystallizes in space group Fm3¯m (no. 225) with the lattice parameters a=7.9903(4) Å, V=510.14(4) Å 3. Its crystal structure was refined on the basis of powder as well as single crystal data. The single crystal refinement converged to R1=0.0239 and w R2=0.0624 for all 88 unique reflections and 6 parameters. Zr 2Ir 6B is isotypic to Ti 2Rh 6B and its structure can be described as a defect double perovskite, A2BB' O6, where the A site is occupied by zirconium, the B site by boron, the O site by iridium but the B' site is vacant, leading to the formation of empty and boron-filled octahedral Ir 6 clusters. According to the result of tight-binding electronic structure calculations, Ir-B and Ir-Zr interactions are mainly responsible for the structural stability of the phase. According to COHP bonding analysis, the strongest bonding occurs for the Ir-B contacts, and the Ir-Ir bonding within the empty clusters is two times stronger than that in the BIr 6 octahedra.

Synthesis, characterization and anti-microbial activity of pure, Cu2+ and Cd2+ doped organic NLO l-arginine trifluoroacetate single crystals

NASA Astrophysics Data System (ADS)

Prasanyaa, T.; Haris, M.; Jayaramakrishnan, V.; Amgalan, M.; Mathivanan, V.

2013-10-01

Optically transparent Cu2+ and Cd2+ doped l-arginine trifluoroacetate (LATF) single crystals were grown from its aqueous solution using the slow solvent evaporation technique. The grown crystals were characterized by powder x-ray diffraction to confirm the monoclinic crystal structure. The percentage of transmittance measured using the ultraviolet-visible-near infrared spectrophotometer was found to be more than 80% for doped crystals. The functional group analysis of the grown crystals has been made by Fourier transform infrared spectroscopy. Thermogravimetric/differential thermal analysis was performed for the grown crystals. An atomic absorption study was carried out to determine the presence of Cu2+ and Cd2+. The hardness of the grown crystals was assessed and the results show a significant variation in the hardness value between the pure and doped LATF crystals. The second harmonic generation measurements show that Cu2+ doped LATF is 2.8 times greater and Cd2+ doped is 2.6 times greater than KDP. The anti-bacterial and anti-fungal activities of the title compound were performed using the disc diffusion method against standard bacteria Escherichia coli, Xanthomonas oryzae and against the fungus Aspergillus niger and Aspergillus flavus.

Yb3+-doped cadmium molybdato-tungstate single crystal - Its structural, optical, magnetic and transport properties

NASA Astrophysics Data System (ADS)

Groń, T.; Tomaszewicz, E.; Berkowski, M.; Głowacki, M.; Oboz, M.; Kusz, J.; Sawicki, B.; Kukuła, Z.; Duda, H.

2018-06-01

Single crystal of new cadmium and ytterbium molybdato-tungstate (Cd0.9706⎕0.0098Yb0.0196(MoO4)0.9706(WO4)0.0294, where ⎕ denotes cationic vacancies) has been successfully grown by the Czochralski method in air and under 1 MPa. X-ray crystallographic analysis reveals that the as-grown single crystal belongs to a scheelite-type structure (a = b = 5.15539(12) and c = 11.1919(3) Å, space group I41/a), in which Yb3+ ions do not show long-range order and are randomly distributed in the unit cell, substituting the Cd2+ ones. The as-grown single crystal does not show anisotropy of optical properties, i.e. its direct band gap reaches Eg = 1.76 or 1.75 eV along (100) and (001) crystallographic directions, respectively. The single crystal exhibits paramagnetic state with short-range antiferromagnetic and long-range ferrimagnetic interactions, a magnetization with zero coercivity and, a remanence that is almost a universal function of H/T, characterizing superparamagnetic-like behaviour. Electrical studies of the new ytterbium-doped cadmium molybdato-tungstate single crystal show a relatively small dielectric constant (εr<12), large lossiness of Joule-Lenz type observed at low frequencies as well as nonlinear I-V characteristics of Schottky or Maxwell-Wagner type.

Single crystal growth and characterization of pure and sodium-modified copper tartrate

NASA Astrophysics Data System (ADS)

Quasim, I.; Firdous, A.; Want, B.; Khosa, S. K.; Kotru, P. N.

2008-12-01

Single crystal growth of pure and modified copper tartrate crystals bearing composition (Cu) x(Na) yC 4H 4O 6· nH 2O (where x=1, 0.77, 0.65; y=0, 0.23, 0.35) is achieved using gel technique. The optimum conditions required for the growth of these crystals are worked out. The morphological development of these crystals is studied using optical and scanning electron microscopy. The dominant habit faces of the grown copper tartrate crystals are (0 0 1) and (1 1 1). Calculation of the cell parameters using CRYSFIRE software suggests that the pure copper tartrate crystal belongs to orthorhombic system with space group P2 1/c whereas the modified copper tartrate falls under tetragonal system with the space group P4 2/nbc. The external morphological development is shown to remain unaffected in the modified copper tartrate. The stoichiometric composition of the crystals is established by EDAX analysis, CH analysis, FTIR spectroscopy and thermoanalytical techniques. Thermal analysis of the grown crystals suggests that pure copper tartrate is thermally stable up to 42.84 °C whereas the modified copper tartrate crystals are stable only up to 33.11 and 25.11 °C. Calculation of the percentage weight loss from the thermogram supplemented by EDAX/CH analysis and FTIR spectroscopy suggest that the chemical formula of pure copper tartrate crystal is CuC 4H 4O 6·3H 2O whereas the chemical formula for the modified copper tartrate crystals is (Cu) 0.77(Na) 0.23C 4H 4O 6·3H 2O and (Cu) 0.65(Na) 0.35 C 4H 4O 6·H 2O.

Growth, structural, optical, thermal and mechanical properties of cytosinium hydrogen selenite: A novel nonlinear optical single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jaikumar, P.; Sathiskumar, S.; Balakrishnan, T., E-mail: balacrystalgrowth@gmail.com

Highlights: • Growth of bulk single crystals of cytosinium hydrogen selenite (CHS) is reported. • Dielectric constant of CHS is measured as a function of Frequency and temperature. • Lower cut off value of UV–vis-NIR spectrum of CHS crystal is observed at 210 nm. • Meyer’s index value of CHS crystal calculated identifies it as a soft material. • Powder SHG efficiency of CHS is about 1.5 times that of KDP crystal. - Abstract: A novel nonlinear optical single crystal of cytosinium hydrogen selenite was grown from aqueous solution of cytosinium hydrogen selenite by slow solvent evaporation method at roommore » temperature. The structural properties of grown crystal have been studied by single crystal and powder X-ray diffraction analysis. Presence of various functional groups was identified from Fourier transform infrared spectroscopy. The optical transmittance and absorbance spectra were recorded by UV–vis-NIR spectrometer and the grown crystal possesses good transparency in the entire visible region. The dielectric constant and dielectric loss of the crystal were calculated as a function of frequency at different temperatures. The mechanical strength of the cytosinium hydrogen selenite crystal was estimated using Vicker’s microhardness tester. Etch patterns of the cytosinium hydrogen selenite crystal were obtained using distilled water as etchant for different etching time. Second harmonic generation efficiency tested using Nd:YAG laser is about 1.5 times that of KDP.« less

Polychromatic Microdiffraction Analysis of Defect Self-Organization in Shock Deformed Single Crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barabash, Rozaliya; Ice, Gene E; Liu, Wenjun

A spatially resolved X-ray diffraction method - with a submicron 3D resolution together with SEM and OIM analysis are applied to understand the arrangements of voids, geometrically necessary dislocations and strain gradient distributions in samples of Al (1 2 3) and Cu (0 0 1) single crystals shocked to incipient spallation fracture. We describe how geometrically necessary dislocations and the effective strain gradient alter white beam Laue patterns of the shocked materials. Several distinct structural zones are observed at different depths under the impact surface. The density of geometrically necessary dislocations (GNDs) is extremely high near the impact and backmore » surface of the shock recovered crystals. The spall region is characterized by a large density of mesoscale voids and GNDs. The spall region is separated from the impact and back surfaces by compressed regions with high total dislocation density but lower GNDs density. Self-organization of shear bands is observed in the shock recovered Cu single crystal.« less

Growth, structural, thermal, dielectric and nonlinear optical properties of potassium hexachloro cadmate (IV) a novel single crystal

NASA Astrophysics Data System (ADS)

Umarani, P.; Jagannathan, K.

2018-02-01

The Potassium hexachloro cadmate (IV) (PHC) single crystal was grown from the aqueous of the solution by a controlled evaporation method. Single crystal XRD solved the structure. FTIR is used to identify the functional groups of grown crystal. The UV-Vis-NIR spectrometer was used to find out the UV cut off region and to calculate the optical band gap of the Potassium hexachloro cadmate (IV) single crystal. The EDAX spectrum has been used to identify the compounds present in title compound. The TG-DTA profile shows the thermal stability of the grown crystal of Potassium hexachloro cadmate (IV). The Vicker's hardness measurement was used to calculate the material hardness of the title compound. The dielectric loss and constant varied with frequencies and activation energy is also calculated. The solid state parameters like plasma energy, Penn gap, Fermi energy, electronic polarizability using Penn analysis and Clausius-Mossotti equation were also calculated for the title compound. The Z-scan technique is used to calculate the third order nonlinear susceptibility of a real and imaginary part.

Influence of VO2+ ions on structural and optical properties of potassium succinate-succinic acid single crystal for non-linear optical applications

NASA Astrophysics Data System (ADS)

Juliet sheela, K.; Subramanian, P.

2018-04-01

A transparent and good optical quality semi organic single crystal of vanadium doped potassium succinate-succinic acid (KSSA) was synthesized by slow evaporation technique at room temperature. The structural perfection was supported by the powder XRD of the KSSA-VO2+ single crystal. Optical behavior of the material was discovered from the absorption and transmission spectra of UV-vis-NIR characterization. Functional group and presence of metal ion in the specimen are depicted from FTIR traces. From the photoluminescence studies, emission of wavelength in the violet region (418 nm) at the excitation of 243 nm could be ascertained. EDAX, SEM measurements identify presence of elements and pictures the step-line growth and the imperfection presents in the grown crystal. EPR analysis extracts the information about the local site symmetry around the impurity ion, molecular orbital coefficients, admixture coefficients and ground state wave function of VO2+ doped KSSA single crystal. Second harmonic generation (SHG) efficiency of the grown crystal was investigated to explore the NLO characteristic of the material.

Investigation of inorganic nonlinear optical potassium penta borate tetra hydrate (PPBTH) single crystals grown by slow evaporation method

NASA Astrophysics Data System (ADS)

Arivuselvi, R.; Babu, P. Ramesh

2018-03-01

Borates family crystals were plays vital role in the field of non linear optics (NLO) due to needs of wide range of applications. In this report, NLO crystals (potassium penta borate tetra hydrate (KB5H8O12) are grown by slow evaporation method at room temperature (28° C) and studied their physical properties. The harvested single crystals are transparent with the dimension of 12 × 10 × 6 mm3 and colourless. X-ray diffraction of single crystals reveals that the grown crystal belongs to orthorhombic system with non-centrosymmetric space group Pba2. All the absorbed functional groups are present in the order of inorganic compounds expect 1688 cm-1 because of water (Osbnd H sbnd O blending) molecule present in the pristine. Crystals show transparent in the entire visible region with 5.9 eV optical band gap and also it shows excellence in both second and third order nonlinear optical properties. Crystals can withstand upto 154 °C without any phase changes which is observed using thermal (TGA/DTA) analysis.

Thermal and Structural Analysis of a Hollow Core Space Shuttle Main Engine (SSME) Turbine Blade

NASA Technical Reports Server (NTRS)

Abdul-Aziz, Ali; Kalluri, Sreeramesh; McGaw, Michael A.

1995-01-01

The influence of primary and secondary orientations on the elastic response of a hollow core, (001)-oriented nickel base single-crystal superalloy turbine blade, was investigated under combined thermal and mechanical conditions. Finite element techniques is employed through MARC finite element code to conduct the analyses on a hollow core SSME turbine blade made out of PWA 1480 single crystal material. Primary orientation of the single crystal superalloy was varied in increments of 2 deg, from 0 to 10 deg, from the (001) direction. Two secondary orientations (0 and 45 deg) were considered with respect to the global coordinate system, as the primary orientation angle was varied. The stresses developed within the single crystal blade were determined for different orientations of the blade. The influence of angular offsets such as the single crystal's primary and secondary orientations and the loading conditions on the elastic stress response of the PWA 1480 hollow blade are summarized. The influence of he primary orientation angle, when constrained between the bounds considered, was not found to be as significant as the influence of the secondary orientation angle.

Crystal growth, structural, optical, thermal, mechanical, laser damage threshold and electrical properties of triphenylphosphine oxide 4-nitrophenol (TP4N) single crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Karuppasamy, P.; Senthil Pandian, Muthu; Ramasamy, P.; Verma, Sunil

2018-05-01

The optically good quality single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) with maximum dimension of 15 × 10 × 5 mm3 were grown by slow evaporation solution technique (SEST) at room temperature. The cell dimensions of the grown TP4N crystal were confirmed by single crystal X-ray diffraction (SXRD) and the crystalline purity was confirmed and planes were indexed by powder X-ray diffraction (PXRD) analysis. Functional groups of TP4N crystal were confirmed by Fourier transform infrared (FTIR) spectral analysis. The optical transmittance of the grown crystal was determined by the UV-Vis NIR spectral analysis and it has good optical transparency in the entire visible region. The band tail (Urbach) energy of the grown crystal was analyzed and it appears to be minimum, which indicates that the TP4N has good crystallinity. The position of valence band (Ev) and conduction band (Ec) of the TP4N have been determined from the electron affinity energy (EA) and the ionization energy (EI) of its elements and using the optical band gap. The thermal behaviour of the grown crystal was investigated by thermogravimetric and differential thermal analysis (TG-DTA). Vickers microhardness analysis was carried out to identify the mechanical stability of the grown crystal and their indentation size effect (ISE) was explained by the Meyer's law (ML), Hays-Kendall's (HK) approach, proportional specimen resistance (PSR) model, modified PSR model (MPSR), elastic/plastic deformation (EPD) model and indentation induced cracking (IIC) model. Chemical etching study was carried out to find the etch pit density (EPD) of the grown crystal. Laser damage threshold (LDT) value was measured by using Nd:YAG laser (1064 nm). The dielectric permittivity (ε՛) and dielectric loss (tan δ) as a function of frequency was measured. The electronic polarizability (α) of the TP4N crystal was calculated. It is well matched to the value which was calculated from Clausius-Mossotti relation, Lorentz-Lorentz equation, optical band gap and coupled dipole method (CDM). The Z-scan technique was carried out using solid state laser (640 nm) to analyze the nonlinear optical properties of the TP4N crystal. It exhibits the self-defocusing and saturable absorbance effect during analysis of closed and open aperture respectively. The nonlinear optical parameters such as refractive index (n2), absorption coefficient (β) and the third order nonlinear optical susceptibility (χ(3)) were analyzed.

Structural, thermal and optical properties of a semiorganic nonlinear optical single crystal: glycine zinc sulphate.

PubMed

Balakrishnan, T; Ramamurthi, K

2007-10-01

Glycine zinc sulphate salt was synthesized and the solubility and metastable zonewidth were estimated from the aqueous solution. Single crystals of glycine zinc sulphate were grown by solvent evaporation method from aqueous solution. Grown crystals were characterized by X-ray diffraction and FT-IR spectral analyses. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. Thermal properties of the crystal were investigated by thermogravimetric analysis. Microhardness study was carried out on (01-1) face of the grown crystal. Its powder second harmonic generation efficiency was measured using Nd:YAG laser and the value was observed to be 0.7 times that of potassium dihydrogen orthophosphate.

Absolute configuration and crystal packing chirality for three conglomerate-forming ortho-halogen substituted phenyl glycerol ethers

NASA Astrophysics Data System (ADS)

Bredikhin, Alexander A.; Gubaidullin, Aidar T.; Bredikhina, Zemfira A.

2010-06-01

Three conglomerate-forming ortho-Hal (Hal = Cl, Br, I) substituted phenyl glycerol ethers 1- 3 were investigated by single-crystal X-ray analysis, and the absolute configuration for all substances was established. The molecular structures and crystal packing details for halogen derivatives were compared with the same characteristics for ortho-OCH 3 and ortho-CH 3 analogues. Two different types of crystal packing were evaluated for these very much alike compounds. The interplay of the supramolecular crystal organization chirality sense and the single molecule absolute configuration was demonstrated. Some stabilizing and destabilizing interactions involving the ortho-substituents were revealed. The resolution of rac-2 by entrainment procedure was successfully realized.

Phenylacetic acid co-crystals with acridine, caffeine, isonicotinamide and nicotinamide: Crystal structures, thermal analysis, FTIR spectroscopy and Hirshfeld surface analysis

NASA Astrophysics Data System (ADS)

Amombo Noa, Francoise M.; Jacobs, Ayesha

2017-07-01

Co-crystals of phenylacetic acid (PAA) with acridine (ACR), caffeine (CAF), isonicotinamide (INM) and nicotinamide (NAM) have been successfully prepared and characterised by single crystal X-ray diffraction, FTIR spectroscopy, thermal analysis and Hirshfeld surface analysis. The ACR, INM and NAM co-crystals with PAA exhibit the carboxylic acid-pyridine heterosynthon. Furthermore the amide-amide supramolecular homosynthon is observed in the PAA co-crystals with INM and NAM as well as Nsbnd H⋯O interactions between the acid and the respective base. The CAF co-crystal exhibits hydrogen bonding between the imidazole nitrogen and the COOH group of the PAA. The compounds demonstrate different stoichiometries; for PAA·ACR and PAA·INM a 1:1 ratio is displayed, a 2:1 in 2PAA·CAF and a 2:2 in the case of 2PAA·2NAM.

Studies on the structural, optical and dielectric properties of samarium coordinated with salicylic acid single crystal

NASA Astrophysics Data System (ADS)

Singh, Harjinder; Slathia, Goldy; Gupta, Rashmi; Bamzai, K. K.

2018-04-01

Samarium coordinated with salicylic acid was successfully grown as a single crystal by low temperature solution technique using mixed solvent of methanol and water in equal ratio. Structural characterization was carried out by single crystal X-ray diffraction analysis and it crystallizes in centrosymmetric space group P121/c1. FTIR and UV-Vis-NIR spectroscopy confirmed the compound formation and help to determine the mode of binding of the ligand to the rare earth-metal ion. Dielectric constant and dielectric loss have been measured over the frequency range 100 Hz - 30MHz. The decrease in dielectric constant with increases in frequency is due to the transition from interfacial polarization to dipolar polarization. The small value of dielectric constant at higher frequency ensures that the crystal is good candidate for NLO devices. Dielectric loss represents the resistive nature of the material.

Growth, spectral, optical, thermal, and mechanical behaviour of an organic single crystal: Quinolinium 2-carboxy 6-nitrophthalate monohydrate

NASA Astrophysics Data System (ADS)

Mohana, J.; Ahila, G.; Bharathi, M. Divya; Anbalagan, G.

2016-09-01

Organic single crystals of quinolinium 2-carboxy 6-nitrophthalate monohydrate (QN) were grown by slow evaporation solution growth technique using ethanol and water as a mixed solvent. X-ray powder diffraction analysis revealed that the crystal belongs to the monoclinic crystal system with space group of P21/c. The functional groups present in the crystallized material confirmed its molecular structure. The optical transparency range and the lower cutoff wavelength were identified from the UV-vis spectrum. The optical constants were determined by UV-visible transmission spectrum at normal incidence, measured over the 200-700 nm spectral range. The dispersion of the refractive index was discussed in terms of the single-oscillator Wemple and DiDomenico model. The calculated HOMO and LUMO energies show that the charge transfer occur within the molecule. Electronic excitation properties were discussed within the framework of two level model on the basis of an orbital analysis. The nonlinear optical absorption coefficient (β) and nonlinear refraction (n2) of QN was measured by Z-scan technique and reported here. Thermal stability of QN was determined using TGA/DSC curves. Vicker's microhardness studies were carried out on the (1 1 ̅0) plane to understand the mechanical properties of the grown crystal. The microhardness measurements showed a Vickers hardness value as 18.4 kg/mm2 which is comparable to well-known organic crystal, urea.

Synthesis, spectral characterization, and single crystal structure studies of (2-nitro-ethene-1,1-diyl)-bis-((4-isopropyl-benzyl)sulfane)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sakthikumar, L., E-mail: lsakthisbk@gmail.com; Mahalakshmy, R.; Bhargavi, G.

2015-12-15

The title compound (2-nitro-ethene-1,1-diyl)-bis-(4-isopropylbenzyl)sulfane) (5), was synthesised using a two step process. The structure of the product (5) was established by UV, FT-IR, {sup 1}H NMR, {sup 13}C NMR, C,H,N analysis, LC-MS and single crystal X-ray diffraction analysis. The single crystal of the title compound (5) was crystallized in Monoclinic with the space group of P21/c. The crystal exhibit the following unit cell parameters a = 12.8165(18), b = 6.1878(6), c = 27.082(4) Å, β = 90.705(17)°, V = 2147.6(5) A{sup 3}, Z = 4, D{sub x} = 1.242 Mg/m{sup 3} and the molecular formula of C{sub 22}H{sub 27}N{sub 1}O{submore » 2}S{sub 2} was found. The final R value was 0.0776. The crystal structure is stabilized by an interesting intramolecular push and pull five membered electrocyclic interaction between the O1–N1–C2–C1–S1- and via the intermolecular H-bonding interaction between C2–H2···O2.« less

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

Growth and characterization of high-purity SiC single crystals

NASA Astrophysics Data System (ADS)

Augustine, G.; Balakrishna, V.; Brandt, C. D.

2000-04-01

High-purity SiC single crystals with diameter up to 50 mm have been grown by the physical vapor transport method. Finite element analysis was used for thermal modeling of the crystal growth cavity in order to reduce stress in the grown crystal. Crystals are grown in high-purity growth ambient using purified graphite furniture and high-purity SiC sublimation sources. Undoped crystals up to 50 mm in diameter with micropipe density less than 100 cm -2 have been grown using this method. These undoped crystals exhibit resistivities in the 10 3 Ω cm range and are p-type due to the presence of residual acceptor impurities, mainly boron. Semi-insulating SiC material is obtained by doping the crystal with vanadium. Vanadium has a deep donor level located near the middle of the band gap, which compensates the residual acceptor resulting in semi-insulating behavior.

Nucleation kinetics, crystal growth and optical studies on lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

Chandran, Senthilkumar; Paulraj, Rajesh; Ramasamy, P.

2017-06-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution technique at 40 °C. The nucleation parameters such as critical radius, interfacial tension, and critical free energy change have been evaluated using the experimental data. The solubility and the nucleation curve of the crystal at different temperatures have been analyzed. The crystal has a positive temperature coefficient of solubility. The metastable zone width and induction period have been determined for the aqueous solution growth of lithium hydrogen oxalate monohydrate. The UV-vis-NIR spectrum showed this crystal has high transparency. The photoconductivity studies indicate lithium hydrogen oxalate monohydrate has positive photoconductivity behaviour. The low etch pit density observed on (0 0 1) crystal surface and the high resolution x-ray difraction analysis indicate the good quality of the grown crystals

Polarization-resolved second-harmonic generation microscopy as a method to visualize protein-crystal domains

PubMed Central

DeWalt, Emma L.; Begue, Victoria J.; Ronau, Judith A.; Sullivan, Shane Z.; Das, Chittaranjan; Simpson, Garth J.

2013-01-01

Polarization-resolved second-harmonic generation (PR-SHG) microscopy is described and applied to identify the presence of multiple crystallographic domains within protein-crystal conglomerates, which was confirmed by synchrotron X-ray diffraction. Principal component analysis (PCA) of PR-SHG images resulted in principal component 2 (PC2) images with areas of contrasting negative and positive values for conglomerated crystals and PC2 images exhibiting uniformly positive or uniformly negative values for single crystals. Qualitative assessment of PC2 images allowed the identification of domains of different internal ordering within protein-crystal samples as well as differentiation between multi-domain conglomerated crystals and single crystals. PR-SHG assessments of crystalline domains were in good agreement with spatially resolved synchrotron X-ray diffraction measurements. These results have implications for improving the productive throughput of protein structure determination through early identification of multi-domain crystals. PMID:23275165

Anisotropy of Single-Crystal Silicon in Nanometric Cutting.

PubMed

Wang, Zhiguo; Chen, Jiaxuan; Wang, Guilian; Bai, Qingshun; Liang, Yingchun

2017-12-01

The anisotropy exhibited by single-crystal silicon in nanometric cutting is very significant. In order to profoundly understand the effect of crystal anisotropy on cutting behaviors, a large-scale molecular dynamics model was conducted to simulate the nanometric cutting of single-crystal silicon in the (100)[0-10], (100)[0-1-1], (110)[-110], (110)[00-1], (111)[-101], and (111)[-12-1] crystal directions in this study. The simulation results show the variations of different degrees in chip, subsurface damage, cutting force, and friction coefficient with changes in crystal plane and crystal direction. Shear deformation is the formation mechanism of subsurface damage, and the direction and complexity it forms are the primary causes that result in the anisotropy of subsurface damage. Structurally, chips could be classified into completely amorphous ones and incompletely amorphous ones containing a few crystallites. The formation mechanism of the former is high-pressure phase transformation, while the latter is obtained under the combined action of high-pressure phase transformation and cleavage. Based on an analysis of the material removal mode, it can be found that compared with the other crystal direction on the same crystal plane, the (100)[0-10], (110)[-110], and (111)[-101] directions are more suitable for ductile cutting.

Optical and chemical analysis of iron in Luna 20 plagioclase.

NASA Technical Reports Server (NTRS)

Bell, P. M.; Mao, H. K.

1973-01-01

Review of analytical data on the iron content of Luna 20 anorthitic plagioclase, obtained by a highly sensitive technique for measuring polarized absorption related to crystal-field splittings and by automated electron microprobe analysis of oriented single crystals. The iron content is found to range from a few hundredths to a few tenths of a weight per cent from crystal to crystal. The optical and chemical properties of the iron appear to be caused by postcrystallization migration and exsolution. Postcrystallization effects may obscure evidence of the original oxidation state and iron concentration of these crystals.

Synthesis, structure and characterization of a hybrid centrosymmetric material (4-dimethylaminopyridinium nitrate gallic acid monohydrate) well-designed for non-linear optics

NASA Astrophysics Data System (ADS)

Ennaceur, Nasreddine; Jalel, Boutheina; Henchiri, Rokaya; Cordier, Marie; Ledoux-Rak, Isabelle

2018-01-01

Hybrid material: 4-Dimethylaminopyridinium nitrate gallic acid monohydrate abbreviated DNGA monohydrate has been successfully synthesized by slow evaporation method at room temperature. X-ray diffraction (XRD) on a single crystal showed that the latter was crystallized in P-1 space group. Likewise, thermal analyses demonstrated the stability of our crystal up to 80 °C. Besides, the analysis of the infrared spectrum (FTIR), allowed us to confirm the presence of the different groups present in the structure. Furthermore, by studying the UV-Visible spectrum, the transparency of our crystal was proven. Despite the fact that of having a centrosymmetric structure, the nonlinear optical properties of our single crystal, which was tested by Kurtz-Perry technique, proved that its second harmonic generation efficiency was 1.22 times more than that of KDP (potassium dihydrogen phosphate) single crystal. This nonlinear optical behavior of the studied compound was also determined through the calculations of polarizability and first hyperpolarizability values.

Dipicolinate salt of imidazole: Discovering its structure and properties using different experimental methodologies and quantum chemical investigations

NASA Astrophysics Data System (ADS)

Thirumurugan, R.; Anitha, K.

2018-03-01

A novel organic proton transfer complex of imidazolium dipicolinate (ID) has been synthesized and it was grown as single crystals using slow evaporation method. The molecular structure of synthesized compound and vibrational modes of its functional groups were confirmed by (1H and 13C) NMR, FTIR and FT-Raman spectroscopic studies, respectively. Single crystal X-ray diffraction (SCXRD) analysis confirmed the orthorhombic system with noncentrosymmetric (NCS), P212121, space group of grown ID crystal. UV-Vis-NIR spectral study confirmed its high optical transparency within the region of 285-1500 nm. Powder second harmonic generation (SHG) efficiency of ID crystal was confirmed and it was 6.8 times that of KDP crystal. TG-DTA and DSC analysis revealed the higher thermal stability of grown crystal as 249 °C. The dielectric response and mechanical behaviour of grown crystal were studied effectively. Density functional theory calculations were performed to probe the relationship between the structure and its properties including molecular optimization, Mulliken atomic charge distribution, frontier molecular orbital (FMOs) and molecular electrostatic potential map (MEP) analysis and first hyperpolarizability. All these experimental and computational results were discussed in this communication and it endorsed the ID compound as a potential NLO candidate could be employed in optoelectronics device applications in near future.

Optical properties of Sulfur doped InP single crystals

NASA Astrophysics Data System (ADS)

El-Nahass, M. M.; Youssef, S. B.; Ali, H. A. M.

2014-05-01

Optical properties of InP:S single crystals were investigated using spectrophotometric measurements in the spectral range of 200-2500 nm. The absorption coefficient and refractive index were calculated. It was found that InP:S crystals exhibit allowed and forbidden direct transitions with energy gaps of 1.578 and 1.528 eV, respectively. Analysis of the refractive index in the normal dispersion region was discussed in terms of the single oscillator model. Some optical dispersion parameters namely: the dispersion energy (Ed), single oscillator energy (Eo), high frequency dielectric constant (ɛ∞), and lattice dielectric constant (ɛL) were determined. The volume and the surface energy loss functions (VELF & SELF) were estimated. Also, the real and imaginary parts of the complex conductivity were calculated.

Hydrogen bonds directed 2D → 3D interdigitated Cd(II) compound: Synthesis, crystal structure and dual-emission luminescent properties

NASA Astrophysics Data System (ADS)

Yu, Yuanyuan

2017-06-01

A new Cd(II) compound, namely [Cd2(btc)(phen)2Cl]n·n(H2O)·n(DMA) (1, H3btc = 1, 3, 5-benzenetricarboxylic acid, phen = 1,10-phenanthroline, DMA = N,N'-dimethylacetamide) has been synthesized and structurally characterized by single-crystal X-ray diffraction analysis. This compound crystallizes in monoclinic P21/n space group with a = 13.5729(7) Å, b = 20.1049(7) Å, c = 13.9450(6) Å, β = 104.671(4)°, Z = 4. Single-crystal X-ray diffraction analysis reveals that compound 1 features a 2D → 3D interdigitated framework directed by the intermolecular hydrogen bonds. In addition, the luminescent properties of compound 1 were also investigated in the solid state at room temperature.

A novel organic nonlinear optical crystal: Creatininium succinate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thirumurugan, R.; Anitha, K., E-mail: singlecerystalxrd@gmail.ciom

2015-06-24

A novel organic material complex of creatininium succinate (CS) has been synthesized and single crystals were grown by the reaction of creatinine and succinic acid from aqueous solution by employing the technique of slow evaporation at room temperature. The structure of the grown crystal has been elucidated using single crystal X-ray diffraction analysis and the structure was refined by least-squares method to R = 0.027 for 1840 reflections. FT-IR spectral investigation has been carried out to identify the various functional groups in the title compound. UV–Vis transmission was carried out which shows the crystal has a good optical transmittance inmore » the visible region with lower cutoff wavelength around 220 nm. Nonlinear optical property of the crystal was confirmed by Kurtz-Perry powder technique.« less

Effects of a High Magnetic Field on the Microstructure of Ni-Based Single-Crystal Superalloys During Directional Solidification

NASA Astrophysics Data System (ADS)

Xuan, Weidong; Lan, Jian; Liu, Huan; Li, Chuanjun; Wang, Jiang; Ren, Weili; Zhong, Yunbo; Li, Xi; Ren, Zhongming

2017-08-01

High magnetic fields are widely used to improve the microstructure and properties of materials during the solidification process. During the preparation of single-crystal turbine blades, the microstructure of the superalloy is the main factor that determines its mechanical properties. In this work, the effects of a high magnetic field on the microstructure of Ni-based single-crystal superalloys PWA1483 and CMSX-4 during directional solidification were investigated experimentally. The results showed that the magnetic field modified the primary dendrite arm spacing, γ' phase size, and microsegregation of the superalloys. In addition, the size and volume fractions of γ/ γ' eutectic and the microporosity were decreased in a high magnetic field. Analysis of variance (ANOVA) results showed that the effect of a high magnetic field on the microstructure during directional solidification was significant ( p < 0.05). Based on both experimental results and theoretical analysis, the modification of microstructure was attributed to thermoelectric magnetic convection occurring in the interdendritic regions under a high magnetic field. The present work provides a new method to optimize the microstructure of Ni-based single-crystal superalloy blades by applying a high magnetic field.

Investigation on synthesis, growth and characterization of CdIn2S2Se2 single crystal grown by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2017-06-01

CdIn2S2Se2 polycrystalline material has been synthesized by melt oscillation method. Vertical Bridgman method was used to grow a good quality CdIn2S2Se2 single crystal. The crystalline phase and growth orientation were confirmed by powder X-ray diffraction pattern and unit cell parameters were determined by single crystal X-ray diffraction analysis. The structural uniformity of CdIn2S2Se2 was studied using Raman scattering spectroscopy at room temperature. The stoichiometric composition variation along the CdIn2S2Se2 was measured using energy dispersive spectrometry. The transmission spectra of CdIn2S2Se2 single crystal gave 42% transmission in the NIR region. Thermal property of CdIn2S2Se2 has been studied using differential thermal analysis. Thermal diffusivity, specific heat capacity and thermal conductivity were also measured. Electrical property was measured using Hall Effect measurement and it confirms the n-type semiconducting nature. The hardness behavior has been measured using Vickers micro hardness measurement and the indentation size effect has been observed.

Experimental and theoretical investigations of non-centrosymmetric 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R., E-mail: nagaphys@yahoo.com

Graphical abstract: ORTEP diagram of HQDBT. - Highlights: • Single crystal XRD and NMR studies confirm the formation of the title compound. • SHG efficiency was found to be 0.6 times that of KDP. • First-order hyperpolarizability (β) was calculated using HF and B3LYP methods. - Abstract: A novel 8-hydroxyquinolinium dibenzoyl-(L)-tartrate methanol monohydrate crystal has been grown by slow evaporation technique. The single crystal X-ray diffraction analysis has been done for the title compound and is found to crystallize in orthorhombic space group P2{sub 1}2{sub 1}2{sub 1}. The optical absorption cut-off wavelength is found to be 440 nm. The vibrationalmore » analysis has been carried out to assess the functional groups present in the title compound. The molecular structure of the title compound has been confirmed by nuclear magnetic resonance spectroscopy. Thermogravimetric, differential scanning calorimetric and differential thermal analyses reveal the melting point and thermal stability of the title compound. The second harmonic generation efficiency is confirmed by Kurtz–Perry powder technique. Further quantum chemical calculations are performed using Gaussian 03 software.« less

Structural, thermal, optical and nonlinear optical properties of ethylenediaminium picrate single crystals

NASA Astrophysics Data System (ADS)

Indumathi, C.; T. C., Sabari Girisun; Anitha, K.; Alfred Cecil Raj, S.

2017-07-01

A new organic optical limiting material, ethylenediaminium picrate (EDAPA) was synthesized through acid base reaction and grown as single crystals by solvent evaporation method. Single crystal XRD analysis showed that EDAPA crystallizes in orthorhombic system with Cmca as space group. The formation of charge transfer complex during the reaction of ethylenediamine and picric acid was strongly evident through the recorded Fourier Transform Infra Red (FTIR), Raman and Nuclear Magnetic Resonance (NMR) spectrum. Thermal (TG-DTA and DSC) curves indicated that the material possesses high thermal stability with decomposition temperature at 243 °C. Optical (UV-Visible-NIR) analysis showed that the grown crystal was found to be transparent in the entire visible and NIR region. Z-scan studies with intense short pulse (532 nm, 5 ns, 100 μJ) excitations, revealed that EDAPA exhibited two photon absorption behaviour and the nonlinear absorption coefficient was found to be two orders of magnitude higher than some of the known optical limiter like Cu nano glasses. EDAPA exhibited a strong optical limiting action with low limiting threshold which make them a potential candidate for eye and photosensitive component protection against intense short pulse lasers.

Three-dimensional analysis of dislocation multiplication during thermal process of grown silicon with different orientations

NASA Astrophysics Data System (ADS)

Gao, B.; Nakano, S.; Harada, H.; Miyamura, Y.; Kakimoto, K.

2017-09-01

We used an advanced 3D model to study the effect of crystal orientation on the dislocation multiplication in single-crystal silicon under accurate control of the cooling history of temperature. The incorporation of the anisotropy effect of the crystal lattice into the model has been explained in detail, and an algorithm for accurate control of the temperature in the furnace has also been presented. This solver can dynamically track the history of dislocation generation for different orientations during thermal processing of single-crystal silicon. Four orientations, [001], [110], [111], and [112], have been examined, and the comparison of dislocation distributions has been provided.

A microcrystal selection technique in protein crystallization

NASA Astrophysics Data System (ADS)

Han, Qing; Lin, Sheng-Xiang

1996-10-01

The goal of protein crystallization is to obtain high quality single crystals for X-ray diffraction analysis. A new and easy technique was employed to control the number and quality of crystals by eliminating poor microcrystals after the spontaneous nucleation. The process was carried out with two samples: human 17β-hydroxysteroid dehydrogenase (17β-HSD) and hen egg white lysozyme. The present study suggests a useful method for the successful crystal growth of biomacromolecules.

Growth, optical, luminescence, thermal and mechanical behavior of an organic single crystal: 3-Acetyl-2-methyl-4-phenylquinolin-1-ium chloride.

PubMed

Nirosha, M; Kalainathan, S; Sarveswari, S; Vijayakumar, V

2014-04-05

A single crystal of 3-acetyl-2-methyl-4-phenylquinolin-1-ium chloride has grown by slow evaporation solution growth technique using ethanol as solvent. The structural, thermal, optical and mechanical property has studied for the grown crystal. Single crystal XRD revealed that the crystal belongs to monoclinic system with space group P21/c. The presences of Functional groups in the crystallized material have confirmed using the FTIR vibrational spectrum. The optical absorbance spectrum recorded from 190 to 1100nm shows the cut-off wavelength occurs at 371nm. The material shows its transparency in the entire region of the visible spectrum. The photoluminescence spectrum shows the ultraviolet and blue emission in the crystal. Thermogravimetric and differential thermal analysis reveal the thermal stability of the grown crystal. Etching study shows the grown mechanism and surface features of the crystal. Vickers microhardness studies have carried out on the (01-1) plane to understand the mechanical properties of the grown crystal. The hardness of the title compound increases on increasing the load. The Meyer's index number (n), and the stiffness constants for different loads has calculated and reported. Copyright © 2013 Elsevier B.V. All rights reserved.

The density and compositional analysis of titanium doped sapphire single crystal grown by the Czocharlski method

NASA Astrophysics Data System (ADS)

Kusuma, H. H.; Ibrahim, Z.; Othaman, Z.

2018-03-01

Titanium doped sapphire (Ti:Al2O3) crystal has attracted attention not only as beautiful gemstones, but also due to their applications as high power laser action. It is very important crystal for tunable solid state laser. Ti:Al2O3 crystals have been success grown using the Czocharlski method with automatic diameter control (ADC) system. The crystals were grown with different pull rates. The structure of the crystal was characterized with X-Ray Diffraction (XRD). The density of the crystal was measurement based on the Archimedes principle and the chemical composition of the crystal was confirmed by the Energy Dispersive X-ray (EDX) Spectroscopy. The XRD patterns of crystals are showed single main peak with a high intensity. Its shows that the samples are single crystal. The Ti:Al2O3 grown with different pull rate will affect the distribution of the concentration of dopant Ti3+ and densities on the sapphire crystals boules as well on the crystal growth process. The increment of the pull rate will increase the percentage distribution of Ti3+ and on the densities of the Ti:Al2O3 crystal boules. This may be attributed to the speed factor of the pull rate of the crystal that then caused changes in the heat flow in the furnace and then causes the homogeneities is changed of species distribution of atoms along crystal.

Growth, structural, optical and thermal properties of gamma-glycine crystal.

PubMed

Balakrishnan, T; Babu, R Ramesh; Ramamurthi, K

2008-04-01

Single crystals of gamma-glycine were grown from a mixture of glycine, water and lithium bromide. Single crystal X-ray diffraction analysis confirmed the growth of gamma-glycine phase. Presence of various functional groups of gamma-glycine was identified by FTIR spectrum. Optical absorbance spectrum recorded in the wavelength range of UV-vis-NIR revealed that this crystal has good optical transparency in the range 250-1500 nm. Vickers microhardness values were estimated on the prominent (100) face. Thermogravimetric and differential scanning calorimetric analyses were carried out to study the thermal properties of gamma-glycine. Second harmonic generation efficiency of the crystal measured by Kurtz's powder method using Nd:YAG laser is about three times that of KDP.

Estimation of the engineering elastic constants of a directionally solidified superalloy for finite element structural analysis

NASA Technical Reports Server (NTRS)

Abdul-Aziz, Ali; Kalluri, Sreeramesh

1991-01-01

The temperature-dependent engineering elastic constants of a directionally solidified nickel-base superalloy were estimated from the single-crystal elastic constants of nickel and MAR-MOO2 superalloy by using Wells' method. In this method, the directionally solidified (columnar-grained) nickel-base superalloy was modeled as a transversely isotropic material, and the five independent elastic constants of the transversely isotropic material were determined from the three independent elastic constants of a cubic single crystal. Solidification for both the single crystals and the directionally solidified superalloy was assumed to be along the (001) direction. Temperature-dependent Young's moduli in longitudinal and transverse directions, shear moduli, and Poisson's ratios were tabulated for the directionally solidified nickel-base superalloy. These engineering elastic constants could be used as input for performing finite element structural analysis of directionally solidified turbine engine components.

Multiplex CARS spectroscopy of Rochelle salt crystal

NASA Astrophysics Data System (ADS)

Hadjichristov, G. B.; Kircheva, P. P.; Kirov, N.

1996-08-01

An optical four-wave mixing (FWM) described by the nonlinear susceptibility x(3) ( ωas = 2 ωp - ωs) is studied in a single crystal of Rochelle salt (NaKC 4H 4O 6·H 2O). In addition to the coherent anti-Stokes Raman Scattering (CARS) structure, the FWM spectra consist of nonvibrational (background) components. After analysis of the FWM spectra in the range from 1100 to 1450 cm -1, the nonresonant (electronic) susceptibility elements xelzzzz and xelxxxx of Rochelle salt single crystal are estimated.

Computational analysis of heat transfer, thermal stress and dislocation density during resistively Czochralski growth of germanium single crystal

NASA Astrophysics Data System (ADS)

Tavakoli, Mohammad Hossein; Renani, Elahe Kabiri; Honarmandnia, Mohtaram; Ezheiyan, Mahdi

2018-02-01

In this paper, a set of numerical simulations of fluid flow, temperature gradient, thermal stress and dislocation density for a Czochralski setup used to grow IR optical-grade Ge single crystal have been done for different stages of the growth process. A two-dimensional steady state finite element method has been applied for all calculations. The obtained numerical results reveal that the thermal field, thermal stress and dislocation structure are mainly dependent on the crystal height, heat radiation and gas flow in the growth system.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts.

PubMed

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-15

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, crystal structure analysis, molecular docking studies and density functional theory predictions of the local reactive properties and degradation properties of a novel halochalcone

NASA Astrophysics Data System (ADS)

Arshad, Suhana; Pillai, Renjith Raveendran; Zainuri, Dian Alwani; Khalib, Nuridayanti Che; Razak, Ibrahim Abdul; Armaković, Stevan; Armaković, Sanja J.

2017-09-01

In the present study, single crystals of E)-3-(3,5-dichlorophenyl)-1-(4-fluorophenyl)prop-2-en-1-one, were prepared and structurally characterized by single crystal X-ray diffraction analysis. The molecular structure crystallized in monoclinic crystal system with P21/c space group. Sensitivity of the title molecule towards electrophilic attacks has been examined by calculations of average localized ionization energies (ALIE) and their mapping to electron density surface. Further determination of atoms that could be important reactive centres has been performed by calculations of Fukui functions. Sensitivity of title molecule towards autoxidation and hydrolysis mechanisms has been assessed by calculations of bond dissociation energies and radial distribution functions (RDF), respectively. Also, in order to explore possible binding mode of the title compound towards Dihydrofolate reductase enzyme, we have utilized in silico molecular docking to explore possible binding modes of the title compound with the DHFR enzyme.

Synthesis, structural, spectroscopic and optical studies of charge transfer complex salts

NASA Astrophysics Data System (ADS)

Manikandan, Maruthappan; Mahalingam, Thaiyan; Hayakawa, Yasuhiro; Ravi, Ganesan

2013-01-01

New charge transfer molecular complex adducts of picric acid (C6H3N3O7) with triethylamine (C6H15N) and dimethylformamide (HCON(CH3)2) were synthesized successfully for the first time. Chemical composition and stoichiometry of the synthesized complex salts were verified by CHN elemental analysis. Solubility of the complex salts have been determined by gravimetric method and single crystals of two new salts were grown by low temperature solution growth technique. Crystal system, crystalline nature and cell parameters of the grown crystals were determined by single crystal X-ray diffraction (SXRD) and powder X-ray diffraction (PXRD) analyses. The formations of the charge-transfer complex, functional groups and the modes of vibrations have been confirmed by Fourier transform infrared (FTIR) spectroscopy. In order to know the linear and nonlinear optical suitability for device fabrication, UV-Vis (UV) spectral analysis and relative second harmonic generation (SHG) efficiency test were performed for the grown crystals.

Growth, crystalline perfection, spectral and optical characterization of a novel optical material: l-tryptophan p-nitrophenol trisolvate single crystal.

PubMed

Sivakumar, N; Srividya, J; Mohana, J; Anbalagan, G

2015-03-15

l-tryptophan p-nitrophenol trisolvate (LTPN), an organic nonlinear optical material was synthesized using ethanol-water mixed solvent and the crystals were grown by a slow solvent evaporation method. The crystal structure and morphology were studied by single crystal X-ray diffraction analysis. The crystalline perfection of the LTPN crystal was analyzed by high-resolution X-ray diffraction study. The molecular structure of the crystal was confirmed by observing the various characteristic functional groups of the material using vibrational spectroscopy. The cut-off wavelength, optical transmission, refractive index and band gap energy were determined using UV-visible data. The variation of refractive index with wavelength shows the normal behavior. The second harmonic generation of the crystal was confirmed and the efficiency was measured using Kurtz Perry powder method. Single and multiple shot methods were employed to measure surface laser damage of the crystal. The photoluminescence spectral study revealed that the emission may be associated with the radiative recombination of trapped electrons and holes. Microhardness measurements revealed that LTPN belongs to a soft material category. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis, growth, structural characterization, Hirshfeld analysis and nonlinear optical studies of a methyl substituted chalcone

NASA Astrophysics Data System (ADS)

Prabhu, Shobha R.; Jayarama, A.; Chandrasekharan, K.; Upadhyaya, V.; Ng, Seik Weng

2017-05-01

A new chalcone compound (2E)-3-(3-methylphenyl)-1-(4-nitrophenyl)prop-2-en-1-one (3MPNP) with molecular formula C16H13NO3 has been synthesized and crystallized by slow solvent evaporation technique. The Fourier transform infrared, Fourier transform Raman and nuclear magnetic resonance techniques were used for structural characterization. UV-visible absorption studies were carried out to study the transparency of the crystal in the visible region. Differential scanning calorimetry study shows thermal stability of crystals up to temperature 122 °C. Single crystal X-ray diffraction and powder X-ray diffraction techniques were used to study crystal structure and cell parameters. The Hirshfeld surface and 2-D fingerprint analysis were performed to study the nature of interactions and their quantitative contributions towards the crystal packing. The third order non-linear optical properties have been studied using single beam Z-scan technique and the results show that the material is a potential candidate for optical device applications such as optical limiters and optical switches.

Synthesis, structural and spectral characterization of a novel NLO crystal N,N‧-diphenylguanidinium picrate: diacetone solvate

NASA Astrophysics Data System (ADS)

Shanmugavadivu, T.; Dhandapani, M.; Naveen, S.; Lokanath, N. K.

2017-09-01

An organic NLO active material N,N‧-diphenylguanidinium picrate: diacetone solvate (C13H14N3+. C6H2N3O7-. 2C3H6O) (DPGPD) was synthesized and single crystals were grown by slow evaporation-solution growth technique at room temperature. DPGPD crystallizes in monoclinic crystal system with noncentrosymmetric space group, Cc confirmed by single crystal X-ray diffraction analysis. The presence of various functional groups was identified from FT-IR spectral analysis and the proton transfer during the formation of compound was confirmed by NMR spectroscopic techniques. The thermal stability was investigated by TG/DTA analyses. Optical transmittance was measured by UV-Vis-NIR spectroscopy and band gap energy was calculated. Photoluminescence spectrum was used to explore its applicability towards laser diodes. Dielectric property of the material was ascertained at different temperatures and it is found that the grown crystal has higher dielectric constant in low frequencies. Photoconductivity study revealed that DPGPD exhibits positive photoconductivity. SHG property was found to be 0.6 times higher than that of KDP.

Synthesis and structural study of 4-(2-chlorophenyl)-2-ethoxy-5,6,7,8,9,10-hexahydrocycloocta[B]pyridine-3-carbonitrile

NASA Astrophysics Data System (ADS)

Fathima, K. Saiadali; Vasumathi, M.; Anitha, K.

2016-05-01

The novel organic material C20H21ClN2O was synthesized by One-Pot synthesis method and the single crystals were grown by slow evaporation solution growth technique. The crystal structure was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R=0.039 for 2746 reflections. Crystal system of the grown crystal was found to be monoclinic with the space group P21/a and a=9.196(4) Å, b=13.449(4) Å, c=14.818(4) Å, β= 101.542(3)°, V=1795.6(11) Å3 and Z=4. In this crystal structure, cyclooctanone prefers to reside in a chair-boat conformation. The structure is stabilized by attractive molecular force such as CH/π interaction called hydrophobic interaction.

Hydrothermal Synthesis, Crystal Structure, and Photoluminescent Properties of Li[UO2(CH3COO)3]3[Co(H2O)6

NASA Astrophysics Data System (ADS)

AlDamen, Murad A.; Juwhari, Hassan K.; Al-zuheiri, Aya M.; Alnazer, Louy A.

2017-12-01

Single crystal of Li[UO2(CH3COO)3]3[Co(H2O)6] was prepared and found to crystallize in the monoclinic crystal system in the sp. gr. C2/ c, with Z = 2, and unit cell parameters a = 22.1857(15) Å, b = 13.6477(8) Å, c = 15.6921(10) Å, β = 117.842(9)°, V = 4201.3(4) Å3. The crystal was characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and differential scanning calorimetry. The single crystal X-ray diffraction analysis revealed that the crystal has a lamellar structure in which a cobalt hydrate is sandwiched within the Li[UO2(CH3COO)3]3 2- chains. Furthermore, the room temperature photoluminescence spectrum of the complex was investigated in the solid state.

Origin of the defects-induced ferromagnetism in un-doped ZnO single crystals

NASA Astrophysics Data System (ADS)

Zhan, Peng; Xie, Zheng; Li, Zhengcao; Wang, Weipeng; Zhang, Zhengjun; Li, Zhuoxin; Cheng, Guodong; Zhang, Peng; Wang, Baoyi; Cao, Xingzhong

2013-02-01

We clarified, in this Letter, that in un-doped ZnO single crystals after thermal annealing in flowing argon, the defects-induced room-temperature ferromagnetism was originated from the surface defects and specifically, from singly occupied oxygen vacancies denoted as F+, by the optical and electrical properties measurements as well as positron annihilation analysis. In addition, a positive linear relationship was observed between the ferromagnetism and the F+ concentration, which is in support with the above clarification.

GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

DTIC Science & Technology

SINGLE CRYSTALS, CRYSTAL GROWTH), (*CRYSTAL GROWTH, SINGLE CRYSTALS), (*RARE EARTH COMPOUNDS, SINGLE CRYSTALS), EPITAXIAL GROWTH, SODIUM COMPOUNDS, CHLORIDES, VAPOR PLATING, ELECTROSTATIC FIELDS, ENERGY, ATOMIC PROPERTIES , BONDING

Optical and Electrical Properties of Sn-Doped Zinc Oxide Single Crystals

DOE PAGES

Haseman, M. S.; Saadatkia, Pooneh; Warfield, J. T.; ...

2017-11-28

Here, Sn dopant in ZnO may significantly improve the n-type conductivity of ZnO through a characteristic double effect. However, studies on bulk Sn-doped ZnO are rare, and the effect of Sn doping on the optoelectronic properties of bulk ZnO is not well understood. In this work, the effect of Sn doping on the optical and electrical properties of ZnO bulk single crystals was investigated through optical absorption spectroscopy, Hall-effect measurements, and thermoluminescence (TL) spectroscopy. Undoped and Sn-doped ZnO single crystals were grown by chemical vapor transport method and characterized by x-ray diffraction analysis. The Sn doping level in the crystalsmore » was evaluated by inductively coupled plasma mass spectroscopy measurements. Hall-effect measurements revealed an increase in conductivity and carrier concentration with increasing Sn doping, while TL measurements identified a few donor species in the crystals with donor ionization energy ranging from 35 meV to 118 meV. Increasing Sn doping was also associated with a color change of single crystals from colorless to dark blue.« less

Growth and characterization of barium complex of 1,3,5-triazinane-2,4,6-trione in gel: a corrosion inhibiting material

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Babu, K. Rajendra

2018-05-01

Good quality prismatic crystals of industrially applicable corrosion inhibiting barium complex of 1,3,5-triazinane-2,4,6-trione have been grown by conventional gel method. The crystal structure, packing, and nature of bonds are revealed in the single crystal X-ray diffraction analysis. The crystal has a three-dimensional polymeric structure having a triclinic crystal system with the space group P-1. The powder X-ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal are identified by Fourier transform infrared spectroscopy. Elemental analysis confirms the stoichiometry of the elements present in the complex. Thermogravimetric analysis and differential thermal analysis reveal its good thermal stability. The optical properties like band gap, refractive index and extinction coefficient are evaluated from the UV-visible spectral analysis. The singular property of the material, corrosion inhibition efficiency achieved by the adsorption of the sample molecules is determined by the weight loss method.

Second harmonic generation and crystal growth of new chalcone derivatives

NASA Astrophysics Data System (ADS)

Patil, P. S.; Dharmaprakash, S. M.; Ramakrishna, K.; Fun, Hoong-Kun; Sai Santosh Kumar, R.; Narayana Rao, D.

2007-05-01

We report on the synthesis, crystal structure and optical characterization of chalcone derivatives developed for second-order nonlinear optics. The investigation of a series of five chalcone derivatives with the second harmonic generation powder test according to Kurtz and Perry revealed that these chalcones show efficient second-order nonlinear activity. Among them, high-quality single crystals of 3-Br-4'-methoxychalcone (3BMC) were grown by solvent evaporation solution growth technique. Grown crystals were characterized by X-ray powder diffraction (XRD), laser damage threshold, UV-vis-NIR and refractive index measurement studies. Infrared spectroscopy, thermogravimetric analysis and differential thermal analysis measurements were performed to study the molecular vibration and thermal behavior of 3BMC crystal. Thermal analysis does not show any structural phase transition.

One-step fabrication of porous GaN crystal membrane and its application in energy storage

NASA Astrophysics Data System (ADS)

Zhang, Lei; Wang, Shouzhi; Shao, Yongliang; Wu, Yongzhong; Sun, Changlong; Huo, Qin; Zhang, Baoguo; Hu, Haixiao; Hao, Xiaopeng

2017-03-01

Single-crystal gallium nitride (GaN) membranes have great potential for a variety of applications. However, fabrication of single-crystalline GaN membranes remains a challenge owing to its chemical inertness and mechanical hardness. This study prepares large-area, free-standing, and single-crystalline porous GaN membranes using a one-step high-temperature annealing technique for the first time. A promising separation model is proposed through a comprehensive study that combines thermodynamic theories analysis and experiments. Porous GaN crystal membrane is processed into supercapacitors, which exhibit stable cycling life, high-rate capability, and ultrahigh power density, to complete proof-of-concept demonstration of new energy storage application. Our results contribute to the study of GaN crystal membranes into a new stage related to the elelctrochemical energy storage application.

Constitutive and life modeling of single crystal blade alloys for root attachment analysis

NASA Technical Reports Server (NTRS)

Meyer, T. G.; Mccarthy, G. J.; Favrow, L. H.; Anton, D. L.; Bak, Joe

1988-01-01

Work to develop fatigue life prediction and constitutive models for uncoated attachment regions of single crystal gas turbine blades is described. At temperatures relevant to attachment regions, deformation is dominated by slip on crystallographic planes. However, fatigue crack initiation and early crack growth are not always observed to be crystallographic. The influence of natural occurring microporosity will be investigated by testing both hot isostatically pressed and conventionally cast PWA 1480 single crystal specimens. Several differnt specimen configurations and orientations relative to the natural crystal axes are being tested to investigate the influence of notch acuity and the material's anisotropy. Global and slip system stresses in the notched regions were determined from three dimensional stress analyses and will be used to develop fatigue life prediction models consistent with the observed lives and crack characteristics.

Synthesis, crystal structures, spectral, thermal and antimicrobial properties of new Zn(II) 5-iodo- and 5-bromosalicylates

NASA Astrophysics Data System (ADS)

Košická, Petra; Győryová, Katarína; Smolko, Lukáš; Gyepes, Róbert; Hudecová, Daniela

2018-03-01

Two new analogous zinc(II) complexes containing 5-iodo- and 5-bromosalicylate ligands, respectively, were prepared in single-crystal form and characterized by IR spectroscopy, thermal analysis and elemental analysis. The solid-state structures of prepared complexes were determined by single crystal X-ray crystallography. Both complexes are isostructural and their crystal structures composed of neutral molecules [Zn(5-Xsal)2(H2O)2] (where X = Br, I, sal = salicylato). Central Zn(II) atom is in both complexes coordinated by six oxygen atoms, four of which are from two chelate bonded 5-halosalicylates and remaining two from coordinated water molecules. The found chelate binding mode is in line with the Δ values calculated from IR spectral data. Antimicrobial activity of prepared complexes was studied against selected bacteria, yeast and filamentous fungi. Obtained results indicate that 5-iodosalicylate complex is more antimicrobially active than its 5-bromo substituted analogue.

Growth of NBT-BT single crystals by flux method and their structural, morphological and electrical characterizations

NASA Astrophysics Data System (ADS)

Kanuru, Sreenadha Rao; Baskar, K.; Dhanasekaran, R.; Kumar, Binay

2016-05-01

In this paper, one of the important, eco-friendly polycrystalline material, (1-x)(Na0.5Bi0.5)TiO3 (NBT) - xBaTiO3 (BT) of different compositions (x=0.07, 0.06 and 0.05 wt%) around the morphotropic phase boundary (MPB) were synthesized by solid state reaction technique. And the single crystals with 13×7×7 mm3, 12×12×7 mm3 and 10×7×4 mm3 dimensions were grown by self flux method. The morphology, crystal structure and unit-cell parameters have been studied and the monoclinic phase has been identified for 0.07 wt% of BT. Higher BT concentration changes the crystal habit and the mechanism has been studied clearly. Raman spectroscopy at room-temperature confirms the presence of functional groups. The quality of the as grown single crystals was examined by high resolution x-ray diffraction analysis. The dielectric properties of the as grown crystals were investigated in the frequency range of 20 Hz-2 MHz from room temperature to 450 °C. The broad dielectric peak and frequency dispersion demonstrates the relaxor behavior of grown crystals. The dielectric constant (εr), transition temperature (Tm), and depolarization temperature (Td) of the grown crystals are found to be comparatively good. The diffusive factor (γ) from Curie-Weiss law confirms the as grown NBT-BT single crystals are relaxor in nature.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ramadhar, Timothy R.; Zheng, Shao-Liang; Chen, Yu-Sheng

This report describes complete practical guidelines and insights for the crystalline sponge method, which have been derived through the first use of synchrotron radiation on these systems, and includes a procedure for faster synthesis of the sponges. These guidelines will be applicable to crystal sponge data collected at synchrotrons or in-house facilities, and will allow researchers to obtain reliable high-quality data and construct chemically and physically sensible models for guest structural determination. A detailed set of synthetic and crystallographic guidelines for the crystalline sponge method based upon the analysis of expediently synthesized crystal sponges using third-generation synchrotron radiation are reported.more » The procedure for the synthesis of the zinc-based metal–organic framework used in initial crystal sponge reports has been modified to yield competent crystals in 3 days instead of 2 weeks. These crystal sponges were tested on some small molecules, with two being unexpectedly difficult cases for analysis with in-house diffractometers in regard to data quality and proper space-group determination. These issues were easily resolved by the use of synchrotron radiation using data-collection times of less than an hour. One of these guests induced a single-crystal-to-single-crystal transformation to create a larger unit cell with over 500 non-H atoms in the asymmetric unit. This led to a non-trivial refinement scenario that afforded the best Flack x absolute stereochemical determination parameter to date for these systems. The structures did not require the use of PLATON/SQUEEZE or other solvent-masking programs, and are the highest-quality crystalline sponge systems reported to date where the results are strongly supported by the data. A set of guidelines for the entire crystallographic process were developed through these studies. In particular, the refinement guidelines include strategies to refine the host framework, locate guests and determine occupancies, discussion of the proper use of geometric and anisotropic displacement parameter restraints and constraints, and whether to perform solvent squeezing/masking. The single-crystal-to-single-crystal transformation process for the crystal sponges is also discussed. The presented general guidelines will be invaluable for researchers interested in using the crystalline sponge method at in-house diffraction or synchrotron facilities, will facilitate the collection and analysis of reliable high-quality data, and will allow construction of chemically and physically sensible models for guest structural determination.« less

Investigations on structural and photoluminescence mechanism of cerium doped L-Histidine hydrochloride mono hydrate single crystals for optical applications

NASA Astrophysics Data System (ADS)

Rajyalakshmi, S.; Ramachandra Rao, K.; Brahmaji, B.; Samatha, K.; Visweswara Rao, T. K.; Ramakrishna, Y.

2017-02-01

Semi organic nonlinear optical material of Ce3+ ion added L-Histidine hydrochloride monohydrate (LHHC) crystals have been grown successfully by the slow evaporation solution technique (SEST) as well as Sankaranarayanan-Ramasamy (SR) technique. Unit cell data have been measured from the single crystal X-ray diffraction analysis and High resolution X-ray diffraction analysis (HRXRD) study shows relatively a good crystalline perfection. Fourier transform infra-red spectroscopy (FTIR) spectra indicates that the Ce3+ ion is coordinated with carboxylate group of grown crystal. The lower UV-cutoff wavelength of the incorporation of Ce3+ ion in LHHC is 240 nm. The incorporation of Ce3+ ion in the crystal lattice was observed by energy dispersive X-ray analysis (EDAX). The nonlinear optical (NLO) efficiency of SR-grown crystal is 3.7 times greater with respect to potassium dihydrogen phosphate (KDP). We report first-time the photoluminescence (PL) mechanism of emission spectrum, which shows broad band located at 350 nm corresponding to 5d → 4f transition of Ce3+ ion and excited by 250 nm wavelength. The excitation spectrum shows a band at 258 nm due to the 4f → 5d transition of Ce3+ ion. The nature of decay curve of the grown crystal is bi-exponential with a long life time of τ2 is 8.8270 μs.

Spectral, optical, thermal, Hirshfeld, antimicrobial studies and computational calculations of a new organic crystal, 1H-benzo[d]imidazol-3-ium-3,5-dinitrobenzoate

NASA Astrophysics Data System (ADS)

Sathya, K.; Dhamodharan, P.; Dhandapani, M.

2017-06-01

Single crystals of 1H-benzo[d]imidazol-3-ium-3,5-dinitrobenzoate (BDNB) were grown by reacting 3,5-dinitrobenzoic acid and benzimidazole by slow evaporation method. UV-Vis-NIR spectral studies of the BDNB show that the crystal is excellently transparent in entire visible region. Chemically and magnetically equivalent protons in BDNB were identified by 1H NMR technique. The carbon frame work of the molecule was established by 13C NMR spectroscopy. Proton transfer mechanism was confirmed by the presence of N+H group in BDNB by FT-IR spectroscopic technique. TG/DTA analyses confirmed that the crystal is stable up to172 °C. Single crystal XRD analysis was carried out to ascertain the molecular structure and the crystal belongs to monoclinic system with space group P21/c. Computational studies that include optimization of molecular geometry, natural bond analysis, Mulliken population analysis and HOMO-LUMO analysis were performed using B3LYP method at 6-31 g level. The low HOMO-LUMO energy gap of BDNB confirms high reactivity of BDNB. Hirshfeld analysis expose that O⋯H/H⋯O interactions are the prominent interactions. Theoretical calculations indicate that first order hyperpolarizability is 16 times greater than urea. The results show that the BDNB may be used for opto-electronic applications. The antimicrobial and antioxidant analyses shows concentration of the compound increases inhibition activity also increases.

Growth and characterization of Melaminium bis (trichloroacetate) dihydrate

NASA Astrophysics Data System (ADS)

Kanagathara, N.; Renganathan, N. G.; Marchewka, M. K.; Sivakumar, N.; Gayathri, K.; Krishnan, P.; Gunasekaran, S.; Anbalagan, G.

2013-01-01

Single crystals of melaminium bis (trichloroacetate) dihydrate have been grown successfully by slow evaporation solution growth technique at room temperature. Single crystal X-ray diffraction analysis reveals that the compound crystallizes in monoclinic system with non -centrosymmetric space group C2 with lattice parameters a = 17.70 Å, b = 8.44 Å, c = 6.09 Å, α = 90°, β = 100.24°, γ = 90° and V = 900 (Å)3. The UV-Vis transmittance spectrum shows that the crystal has a good optical transmittance in the entire visible region with lower cutoff wavelength of 351 nm. The vibrational frequencies of various functional groups present in the crystal have been derived from FI-IR, FT-Raman and Confocal Raman analyses. The chemical structure of the compound was established by 1H and 13C NMR spectrum. TGA-DTA analysis reveals that the materials have good thermal stability and the melting point of the crystal is found to be 195 °C. The dielectric response of the crystals was studied in the frequency range 50 Hz to 5 MHz at different temperatures and the results are discussed. Etching studies show the growth pattern of the crystals. The second harmonic generation efficiency was measured in comparison with KDP by employing powder Kurtz method.

Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

NASA Technical Reports Server (NTRS)

Arakere, Nagaraj K.; Swanson, Gregory R.

2000-01-01

High Cycle Fatigue (HCF) induced failures in aircraft gas-turbine engines is a pervasive problem affecting a wide range of components and materials. HCF is currently the primary cause of component failures in gas turbine aircraft engines. Turbine blades in high performance aircraft and rocket engines are increasingly being made of single crystal nickel superalloys. Single-crystal Nickel-base superalloys were developed to provide superior creep, stress rupture, melt resistance and thermomechanical fatigue capabilities over polycrystalline alloys previously used in the production of turbine blades and vanes. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493 and PWA 1484. These alloys play an important role in commercial, military and space propulsion systems. PWA1493, identical to PWA1480, but with tighter chemical constituent control, is used in the NASA SSME (Space Shuttle Main Engine) alternate turbopump, a liquid hydrogen fueled rocket engine. Objectives for this paper are motivated by the need for developing failure criteria and fatigue life evaluation procedures for high temperature single crystal components, using available fatigue data and finite element modeling of turbine blades. Using the FE (finite element) stress analysis results and the fatigue life relations developed, the effect of variation of primary and secondary crystal orientations on life is determined, at critical blade locations. The most advantageous crystal orientation for a given blade design is determined. Results presented demonstrates that control of secondary and primary crystallographic orientation has the potential to optimize blade design by increasing its resistance to fatigue crack growth without adding additional weight or cost.

Generalized Reliability Methodology Applied to Brittle Anisotropic Single Crystals. Degree awarded by Washington Univ., 1999

NASA Technical Reports Server (NTRS)

Salem, Jonathan A.

2002-01-01

A generalized reliability model was developed for use in the design of structural components made from brittle, homogeneous anisotropic materials such as single crystals. The model is based on the Weibull distribution and incorporates a variable strength distribution and any equivalent stress failure criteria. In addition to the reliability model, an energy based failure criterion for elastically anisotropic materials was formulated. The model is different from typical Weibull-based models in that it accounts for strength anisotropy arising from fracture toughness anisotropy and thereby allows for strength and reliability predictions of brittle, anisotropic single crystals subjected to multiaxial stresses. The model is also applicable to elastically isotropic materials exhibiting strength anisotropy due to an anisotropic distribution of flaws. In order to develop and experimentally verify the model, the uniaxial and biaxial strengths of a single crystal nickel aluminide were measured. The uniaxial strengths of the <100> and <110> crystal directions were measured in three and four-point flexure. The biaxial strength was measured by subjecting <100> plates to a uniform pressure in a test apparatus that was developed and experimentally verified. The biaxial strengths of the single crystal plates were estimated by extending and verifying the displacement solution for a circular, anisotropic plate to the case of a variable radius and thickness. The best correlation between the experimental strength data and the model predictions occurred when an anisotropic stress analysis was combined with the normal stress criterion and the strength parameters associated with the <110> crystal direction.

Effect of amino acid doping on the growth and ferroelectric properties of triglycine sulphate single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raghavan, C.M.; Sankar, R.; Mohan Kumar, R.

2008-02-05

Effect of amino acids (L-leucine and isoleucine) doping on the growth aspects and ferroelectric properties of triglycine sulphate crystals has been studied. Pure and doped crystals were grown from aqueous solution by low temperature solution growth technique. The cell parameter values were found to significantly vary for doped crystals. Fourier transform infrared analysis confirmed the presence of functional groups in the grown crystal. Morphology study reveals that amino acid doping induces faster growth rate along b-direction leading to a wide b-plane and hence suitable for pyroelectric detector applications. Ferroelectric domain structure has been studied by atomic force microscopy and hysteresismore » measurements reveal an increase of coercive field due to the formation of single domain pattern.« less

Effect of L-aspartic acid on the growth, structure and spectral studies of Zinc (tris) Thiourea Sulphate (ZTS) single crystals

NASA Astrophysics Data System (ADS)

Samuel, Bincy Susan; Krishnamurthy, R.; Rajasekaran, R.

2014-11-01

Single crystals of pure and L-aspartic acid doped Zinc (Tris) Thiourea Sulphate (ZTS) were grown from aqueous solution by solution growth method. The cell parameters and structure of the grown crystals were determined by X-ray diffraction studies. The presence of functional group in the compound has been confirmed by FTIR and FT-Raman analysis. The optical transparency range has been studied through UV-Vis spectroscopy. TGA/DTA studies show thermal stability of the grown crystals. Microhardness study reveals that the hardness number (Hv) increases with load for pure and doped ZTS crystals. Dielectric studies have been carried out and the results are discussed. The second harmonic generation was confirmed for L-aspartic acid doped ZTS which is greater than pure ZTS.

Single Crystal Synthesis and STM Studies of High Temperature Superconductors

NASA Technical Reports Server (NTRS)

Barrientos, Alfonso

1997-01-01

This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

Superposition model analysis of zero field splitting for Mn2+ in some host single crystals

NASA Astrophysics Data System (ADS)

Bansal, R. S.; Ahlawat, P.; Bharti, M.; Hooda, S. S.

2013-07-01

The Newman superposition model has been used to investigate the substitution of Mn2+ for Zn2+ site in ammonium tetra flurozincate dihydrate and for Co2+ site in cobalt ammonium phosphate hexahydrate and cobalt potassium phosphate hexahydrate single crystals. The calculated values of zero field splitting parameter b 2 0 at room temperature fit the experimental data with average intrinsic parameters overline{b}2 (F) = -0.0531 cm-1 for fluorine and overline{b}2 (O) = -0.0280 cm-1 for oxygen, taken t 2 = 7 for Mn2+ doped in ammonium tetra fluorozincate dihydrate single crystals. The values of overline{b}2 determined for Mn2+ doped in cobalt ammonium phosphate hexahydrate are -0.049 cm-1 for site I and -0.045 cm-1 for site II and in cobalt pottasium phosphate hexahydrate single crystals it is found to be overline{b}2 = -0.086 cm-1. We find close agreement between theoretical and experimental values of b 2 0.

Studies on the growth, structural, optical, mechanical properties of 8-hydroxyquinoline single crystal by vertical Bridgman technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prabhakaran, SP.; Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Velusamy, P.

2011-11-15

Highlights: {yields} Growth of bulk single crystal of 8-hydroxyquinoline (8-HQ) by vertical Bridgman technique for the first time. {yields} The crystalline perfection is reasonably good. {yields} The photoluminescence spectrum shows that the material is suitable for blue light emission. -- Abstract: Single crystal of organic nonlinear optical material, 8-hydroxyquinoline (8-HQ) of dimension 52 mm (length) x 12 mm (dia.) was grown from melt using vertical Bridgman technique. The crystal system of the material was confirmed by powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. Low angular spread around 400'' ofmore » the diffraction curve and the low full width half maximum values show that the crystalline perfection is reasonably good. The recorded photoluminescence spectrum shows that the material is suitable for blue light emission. Optical transmittance for the UV and visible region was measured and mechanical strength was estimated from Vicker's microhardness test along the growth face of the grown crystal.« less

Structural, thermal and optical characterization of an organic NLO material--benzaldehyde thiosemicarbazone monohydrate single crystals.

PubMed

Santhakumari, R; Ramamurthi, K

2011-02-01

Single crystals of the organic NLO material, benzaldehyde thiosemicarbazone (BTSC) monohydrate, were grown by slow evaporation method. Solubility of BTSC monohydrate was determined in ethanol at different temperatures. The grown crystals were characterized by single crystal X-ray diffraction analysis to determine the cell parameters and by FT-IR technique to study the presence of the functional groups. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. UV-vis-NIR spectrum shows excellent transmission in the region of 200-1100 nm. Theoretical calculations were carried out to determine the linear optical constants such as extinction coefficient and refractive index. Further the optical nonlinearities of BTSC have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Mechanical properties of the grown crystal were studied using Vickers microhardness tester. Second harmonic generation efficiency of the powdered BTSC monohydrate was tested using Nd:YAG laser and it is found to be ∼5.3 times that of potassium dihydrogen orthophosphate. Copyright © 2010 Elsevier B.V. All rights reserved.

Site selectivity on chalcogen atoms in superconducting La(O,F)BiSSe

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tanaka, Masashi, E-mail: Tanaka.Masashi@nims.go.jp; Matsushita, Yoshitaka; Fujioka, Masaya

2015-03-16

Single crystals of La(O,F)BiSSe were grown by using a CsCl flux method. Single crystal X-ray structural analysis reveals that the crystal structure is isostructural to the BiS{sub 2}- or BiSe{sub 2}-based compounds crystallizing with space group P4/nmm (lattice parameters a = 4.1110(2) Å, c = 13.6010(7) Å). However, the S atoms are selectively occupied at the apical site of the Bi-SSe pyramids in the superconducting layer. The single crystals show a superconducting transition at around 4.2 K in the magnetic susceptibility and resistivity measurements. The superconducting anisotropic parameter is determined to be 34–35 from its upper critical magnetic field. The anisotropy is in the same range withmore » that of other members of the La(O,F)BiCh{sub 2} (Ch = S, Se) family under ambient pressure.« less

The effect of aluminium on mechanical properties and deformation mechanisms of hadfield steel single crystals

NASA Astrophysics Data System (ADS)

Zakharova, E. G.; Kireeva, I. V.; Chumlyakov, Y. I.; Shul'Mina, A. A.; Sehitoglu, H.; Karaman, I.

2004-06-01

On single crystals of Hadfield steel (Fe-13Mn-1.3C, Fe-13Mn-2.7Al-1.3C, wt.%) the systematical investigations of deformation mechanisms - slip and twinning, stages of plastic flow, strain hardening coefficient depending on orientation of tensile axis have been carried out by methods of optical and electron microscopy, x-ray analysis. Is has been shown that the combination of low stacking fault energy (γ{SF}=0.03J/m^2) with high concentration of carbon atoms in aluminium-free steel results in development of the mechanical twinning at room temperature in all crystal orientations. The new type of twinning with formation of extrinsic stacking fault has been found out in [001] single crystals. Experimentally it has been established that alloying with aluminium leads to increase of stacking fault energy of Hadfield steel and suppresses twinning in all orientations of crystals at preservation of high values of strain-hardening coefficients θ.

New supramolecular cocrystal of 2-amino-5-chloropyridine with 3-methylbenzoic acids: Syntheses, structural characterization, Hirshfeld surfaces and quantum chemical investigations

NASA Astrophysics Data System (ADS)

Thanigaimani, Kaliyaperumal; Khalib, Nuridayanti Che; Temel, Ersin; Arshad, Suhana; Razak, Ibrahim Abdul

2015-11-01

2-amino-5-chloropyridine: 3-methylbenzoic acid [(2A5CP) (3MBA)] (I) cocrystal was synthesized and its single crystal was grown by slow evaporation technique. The structure of the grown crystal was elucidated by using single crystal X-ray diffraction technique. The cocrystal belongs to the monoclinic crystallographic system with space group P21/c, Z = 4, and a = 13.3155 (5) Å, b = 5.5980 (2) Å, c = 18.3787 (7) Å, β = 110.045 (2)°. The crystal structure is stabilized by Npyridine-H•••Odbnd C, Cdbnd O-H•••Npyridine and C-H⋯O type hydrogen bonding interactions. The presence of unionized -COOH functional group in the cocrystal was identified both by spectral methods and X-ray structural analysis. The experimental studies obtained by using the methods of single crystal X-ray analysis, powder X-ray diffraction (PXRD) analysis, FTIR, 1H NMR and 13C NMR spectroscopies confirmed the predicted cocrystal. The supramolecular assembly of the cocrystal was analyzed and discussed. The molecular geometry, vibrational frequencies of the compound in the ground state were calculated by using the density functional theory (DFT) method with 6-311++G (d,p) basis set and were compared with the experimental data. Additionally, HOMO-LUMO energy gap, natural bond orbital (NBO) analysis and nonlinear optical (NLO) properties of the compound were performed at B3LYP/6-311++G (d,p) level. Hirshfeld surfaces were used to confirm the existence of inter-molecular interactions in the compound.

Neutralization of Hydroxide Ion in Melt-Grown NaCl Crystals

NASA Technical Reports Server (NTRS)

Otterson, Dumas A.

1961-01-01

Many recent studies of solid-state phenomena, particularly in the area of crystal imperfections, have involved the use of melt-grown NaCl single crystals. Quite often trace impurities in these materials have had a prominent effect on these phenomena. Trace amounts of hydroxide ion have been found in melt-grown NaCl crystals. This paper describes a nondestructive method of neutralizing the hydroxide ion in such crystals. Crystals of similar hydroxide content are maintained at an elevated temperature below the melting point of NaCl in a flowing atmosphere containing. dry hydrogen chloride. Heat treatment is continued until an analysis of the test specimens shows no excess hydroxide ion. A colorimetric method previously described4 is used for this analysis.

Growth, structure, Hirshfeld surface and spectroscopic properties of 2-amino-4-hydroxy-6-methylpyrimidinium-2,3-pyrazinedicorboxylate single crystal

NASA Astrophysics Data System (ADS)

Faizan, Mohd; Alam, Mohammad Jane; Afroz, Ziya; Rodrigues, Vítor Hugo Nunes; Ahmad, Shabbir

2018-03-01

The present work is focused on the crystal structure, vibrational spectroscopy and DFT calculations of hydrogen bonded 2,3-pyrazinedicorboxylic acid and 2-amino-4-hydroxy-6-methylpyrimidine (PDCA-.AHMP+) crystal. The crystal structure has been determined using single crystal X-ray diffraction analysis which shows that the crystal belongs to monoclinic space group P21/n. The PDCA-.AHMP+ crystal has been characterized by FTIR, FT-Raman and FT-NMR spectroscopic techniques. The FTIR and FT-Raman spectra of the complex have unique spectroscopic feature as compared with those of the starting material to confirm salt formation. The theoretical vibrational studies have been performed to understand the modes of the vibrations of asymmetric unit of the complex by DFT methods. Hirschfeld surface and 2D fingerprint plots analyses were carried out to investigate the intermolecular interactions and its contribution in the building of PDCA-.AHMP+ crystal. The experimental and simulated 13C and 1H NMR studies have assisted in structural analysis of PDCA-.AHMP+ crystal. The electronic spectroscopic properties of the complex were explored by the experimental as well as theoretical electronic spectra simulated using TD-DFT/IEF-PCM method at B3LYP/6-311++G (d,p) level of theory. In addition, frontier molecular orbitals, molecular electrostatic potential map (MEP) and nonlinear optical (NLO) properties using DFT method have been also presented.

How the Molecular Packing Affects the Room Temperature Phosphorescence in Pure Organic Compounds: Ingenious Molecular Design, Detailed Crystal Analysis, and Rational Theoretical Calculations.

PubMed

Xie, Yujun; Ge, Yuwei; Peng, Qian; Li, Conggang; Li, Qianqian; Li, Zhen

2017-05-01

Long-lived phosphorescence at room temperature (RTP) from pure organic molecules is rare. Recent research reveals various crystalline organic molecules can realize RTP with lifetimes extending to the magnitude of second. There is little research on how molecular packing affecting RTP. Three compounds are designed with similar optical properties in solution, but tremendously different solid emission characteristics. By investigating the molecular packing arrangement in single crystals, it is found that the packing style of the compact face to face favors of long phosphorescence lifetime and high photoluminescence efficiency, with the lifetime up to 748 ms observed in the crystal of CPM ((9H-carbazol-9-yl)(phenyl)methanone). Theoretical calculation analysis also reveals this kind of packing style can remarkably reduce the singlet excited energy level and prompt electron communication between dimers. Surprisingly, CPM has two very similar single crystals, labeled as CPM and CPM-A, with almost identical crystal data, and the only difference is that molecules in CPM-A crystal take a little looser packing arrangement. X-ray diffraction and cross-polarization under magic spinning 13 C NMR spectra double confirm that they are different crystals. Interestingly, CPM-A crystal shows negligible RTP compared to the CPM crystal, once again proving that the packing style is critical to the RTP property. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystal growth, thermal and optical studies of semiorganic nonlinear optical material: L-lysine hydrochloride dihydrate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kalaiselvi, D.; Mohan Kumar, R.; Jayavel, R.

2008-07-01

Single crystals of L-lysine hydrochloride dihydrate (LLHCD), a nonlinear optical material, have been grown by slow cooling technique from its aqueous solution. LLHCD was found to be highly soluble in water. The grown crystals have been subjected to single crystal X-ray diffraction to confirm the structure and to estimate the lattice parameters. The vibrational structure of the molecule is elucidated from FTIR spectra. Thermal analysis revealed the thermal stability of the grown crystals. The optical transmittance spectrum shows that the material possesses good optical transparency in the entire visible region with a UV cut-off wavelength at 228 nm. The mechanicalmore » properties of the grown crystal have been studied using Vicker's microhardness test. The laser damage threshold of 52.25 MW/cm{sup 2} has been measured by irradiating Q-switched Nd:YAG laser (1064 nm)« less

Single crystal structure analyses of scheelite-powellite CaW1-xMoxO4 solidsolutions and unique occurrence in Jisyakuyama skarn deposits

NASA Astrophysics Data System (ADS)

Yamashita, K.; Yoshiasa, A.; Miyazaki, H.; Tokuda, M.; Tobase, T.; Isobe, H.; Nishiyama, T.; Sugiyama, K.; Miyawaki, R.

2017-12-01

Jisyakuyama skarn deposit, Fukuchi, Fukuoka, Japan, shows a simple occurrenceformed by penetration of hot water into limestone cracks. A unique occurrence of scheelite-powellite CaW1-xMoxO4 minerals is observed in the skarn deposit. Many syntheticexperiments for scheelite-powellite solid solutions have been reported as research onfluorescent materials. In this system it is known that a complete continuous solid solution isformed even at room temperature. In this study, we have carried out the chemical analyses,crystal structural refinements and detail description of occurrence on scheelite-powelliteminerals. We have also attempted synthesis of single crystal of solid solution in a widecomposition range. The chemical compositions were determined by JEOL scanningelectron microscope and EDS, INCA system. We have performed the crystal structurerefinements of the scheelite-powellite CaW1-xMoxO4 solid solutions (x=0.0-1.0) byRIGAKU single-crystal structure analysis system RAPID. The R and S values are around0.0s and 1.03. As the result of structural refinements of natural products and many solidsolutions, we confirm that most large natural single crystals have compositions at bothendmembers, and large solid solution crystals are rare. The lattice constants, interatomicdistances and other crystallographic parameters for the solid solution change uniquely withcomposition and it was confirmed as a continuous solid solution. Single crystals of scheeliteendmember + powellite endmember + solid solution with various compositions form anaggregate in the deposit (Figure 1). Crystal shapes of powellite and scheelite arehypidiomorphic and allotriomorphic, respectively. Many solid solution crystals areaccompanied by scheelite endmember and a compositional gap is observed betweenpowellite and solid-solution crystals. The presence of several penetration solutions withsignificantly different W and Mo contents may be assumed. This research can be expectedto lead to giving restrictive conditions to elucidate the mineralization process. Figure1. Scheelite + Powellite + solid solution aggregate

Hydrothermal syntheses, crystal structures, and photophysical properties of two coordination polymers with mixed ligands

NASA Astrophysics Data System (ADS)

Yan, Li; Liu, Chun-Ling

2017-10-01

Two novel metal-organic coordination polymers [Cd(ipdt)(m-BDC)·3H2O]n (1) and [Pb(mip)2(NTC) ·2H2O]n (2) [ipdt = 2,6-Dimethoxy-4-(1H-1,3,7,8-tetraaza-cyclopenta[l]phenanthren-2-yl)-phenol, mip = 2-(3-methoxyphenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, m-BDC = isophthalic acid, NTC = nicotinic acid] have been synthesized by hydrothermal reactions and characterized by elemental analysis, thermogravimetric (TG) analysis, infrared spectrum (IR) and single-crystal X-ray diffraction. Single-crystal X-ray diffraction reveals that 1 exhibits two-dimensional (2D) layer architecture, and 2 shows 1D chain architecture. TG analysis shows clear courses of weight loss, which corresponds to the decomposition of different ligands. The luminescent properties for the ligand ipdt, mip and complexes 1-2 are also discussed in detail, which should be acted as potential luminescent material.

Fabrication and analysis of single-crystal KTiOPO₄ films with thicknesses in the micrometer range.

PubMed

Ma, Changdong; Lu, Fei; Xu, Bo; Fan, Ranran

2016-02-01

Single-crystal potassium titanyl phosphate (KTiOPO4, KTP) films with thicknesses less than 5 μm are obtained by using helium (He) implantation combined with ion-beam-enhanced etching. A heavily damaged layer created by a 4×10(16)  cm(-2) fluence of 2 MeV He implantation is removed by means of wet chemical etching in hydrofluoric acid (HF). Thus, free-standing films of KTP with thicknesses in the range of 3-5 μm are obtained. The etching rate can be adjusted over a wide range by choosing temperature and HF concentration, as well as annealing conditions. Sharp etching edges and the smooth surface of the film indicate that a high selective-etching rate is achieved in the damaged layer, and the remaining part of the crystal is undamaged. X-ray and Raman-scattering results prove that KTP films have good single-crystal properties.

Correlation of the superconducting transition to oxygen stoichiometry in single-crystal Ba1-xKxBiO3-y

NASA Astrophysics Data System (ADS)

Mosley, W. D.; Dykes, J. W.; Klavins, P.; Shelton, R. N.; Sterne, P. A.; Howell, R. H.

1993-07-01

Temperature-dependent positron-lifetime experiments have been performed from room temperature to 15 K on single crystals of the oxide superconductor Ba1-xKxBiO3-y. Results indicate that the filling of oxygen vacancies has a marked impact on the superconducting properties of this system. Cation defect concentrations were below the detectable limit of positron-annihilation-analysis techniques in this material, which is in sharp contrast to identical studies on polycrystalline samples. We find that the positron lifetime in these electrochemically deposited single crystals is determined by the oxygen stoichiometry of the lattice, but there is no experimental signature of strong positron localization. By performing a subsequent oxygen anneal on the crystals, the superconducting transition is sharpened and the onset is raised. The observed change in positron lifetime associated with this annealing procedure is in quantitative agreement with theory.

Quantitative analysis with advanced compensated polarized light microscopy on wavelength dependence of linear birefringence of single crystals causing arthritis

NASA Astrophysics Data System (ADS)

Takanabe, Akifumi; Tanaka, Masahito; Taniguchi, Atsuo; Yamanaka, Hisashi; Asahi, Toru

2014-07-01

To improve our ability to identify single crystals causing arthritis, we have developed a practical measurement system of polarized light microscopy called advanced compensated polarized light microscopy (A-CPLM). The A-CPLM system is constructed by employing a conventional phase retardation plate, an optical fibre and a charge-coupled device spectrometer in a polarized light microscope. We applied the A-CPLM system to measure linear birefringence (LB) in the visible region, which is an optical anisotropic property, for tiny single crystals causing arthritis, i.e. monosodium urate monohydrate (MSUM) and calcium pyrophosphate dihydrate (CPPD). The A-CPLM system performance was evaluated by comparing the obtained experimental data using the A-CPLM system with (i) literature data for a standard sample, MgF2, and (ii) experimental data obtained using an established optical method, high-accuracy universal polarimeter, for the MSUM. The A-CPLM system was found to be applicable for measuring the LB spectra of the single crystals of MSUM and CPPD, which cause arthritis, in the visible regions. We quantitatively reveal the large difference in LB between MSUM and CPPD crystals. These results demonstrate the usefulness of the A-CPLM system for distinguishing the crystals causing arthritis.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rai, R.N., E-mail: rn_rai@yahoo.co.in; Kant, Shiva; Reddi, R.S.B.

Urea is an attractive material for frequency conversion of high power lasers to UV (for wavelength down to 190 nm), but its usage is hindered due to its hygroscopic nature, though there is no alternative organic NLO crystal which could be transparent up to 190 nm. The hygroscopic character of urea has been modified by making the solid solution (UCNB) of urea (U) and p-chloronitrobenzene (CNB). The formation of the solid solution of CNB in U is explained on the basis of phase diagram, powder XRD, FTIR, elemental analysis and single crystal XRD studies. The solubility of U, CNB andmore » UCNB in ethanol solution is evaluated at different temperatures. Transparent single crystals of UCNB are grown from its saturated solution in ethanol. Optical properties e.g., second harmonic generation (SHG), refractive index and the band gap for UCNB crystal were measured and their values were compared with the parent compounds. Besides modification in hygroscopic nature, UCNB has also shown the higher SHG signal and mechanical hardness in comparison to urea crystal. - Highlights: • The hygroscopic character of urea was modified by making the solid solution • Solid solution formation is support by elemental, powder- and single crystal XRD • Crystal of solid solution has higher SHG signal and mechanical stability. • Refractive index and band gap of solid solution crystal have determined.« less

Effect of oxygen on dislocation multiplication in silicon crystals

NASA Astrophysics Data System (ADS)

Fukushima, Wataru; Harada, Hirofumi; Miyamura, Yoshiji; Imai, Masato; Nakano, Satoshi; Kakimoto, Koichi

2018-03-01

This paper aims to clarify the effect of oxygen on dislocation multiplication in silicon single crystals grown by the Czochralski and floating zone methods using numerical analysis. The analysis is based on the Alexander-Haasen-Sumino model and involves oxygen diffusion from the bulk to the dislocation cores during the annealing process in a furnace. The results show that after the annealing process, the dislocation density in silicon single crystals decreases as a function of oxygen concentration. This decrease can be explained by considering the unlocking stress caused by interstitial oxygen atoms. When the oxygen concentration is 7.5 × 1017 cm-3, the total stress is about 2 MPa and the unlocking stress is less than 1 MPa. As the oxygen concentration increases, the unlocking stress also increases; however, the dislocation velocity decreases.

Polymorphism of a new Mannich base - [-4-methyl-2-((4-(4-nitrophenyl)piperazin-1-yl)methyl)phenol

NASA Astrophysics Data System (ADS)

Ayeni, Ayowole O.; Watkins, Gareth M.; Hosten, Eric C.

2018-05-01

Two polymorphs (forms I and II) of a new Mannich base 4-methyl-2-((4-(4-nitrophenyl)piperazin-1-yl)methyl)phenol have been isolated and characterized by single crystal and powder (experimental and theoretical) X-ray diffraction, thermal analysis (differential scanning calorimetry), Fourier transform infrared spectroscopy. 1H and 13C nuclear magnetic resonance spectroscopy was employed in characterising the new Mannich base. Single crystal X-ray diffraction revealed that the two polymorphs contain different conformers of the Mannich base whose hydrogen bonding schemes and packing arrangements in their respective crystals are different. Thermal analysis led to the conclusion that the two polymorphs are enantiotropically related, with a transition temperature of 138.5 °C.

Additive Manufacturing of Single-Crystal Superalloy CMSX-4 Through Scanning Laser Epitaxy: Computational Modeling, Experimental Process Development, and Process Parameter Optimization

NASA Astrophysics Data System (ADS)

Basak, Amrita; Acharya, Ranadip; Das, Suman

2016-08-01

This paper focuses on additive manufacturing (AM) of single-crystal (SX) nickel-based superalloy CMSX-4 through scanning laser epitaxy (SLE). SLE, a powder bed fusion-based AM process was explored for the purpose of producing crack-free, dense deposits of CMSX-4 on top of similar chemistry investment-cast substrates. Optical microscopy and scanning electron microscopy (SEM) investigations revealed the presence of dendritic microstructures that consisted of fine γ' precipitates within the γ matrix in the deposit region. Computational fluid dynamics (CFD)-based process modeling, statistical design of experiments (DoE), and microstructural characterization techniques were combined to produce metallurgically bonded single-crystal deposits of more than 500 μm height in a single pass along the entire length of the substrate. A customized quantitative metallography based image analysis technique was employed for automatic extraction of various deposit quality metrics from the digital cross-sectional micrographs. The processing parameters were varied, and optimal processing windows were identified to obtain good quality deposits. The results reported here represent one of the few successes obtained in producing single-crystal epitaxial deposits through a powder bed fusion-based metal AM process and thus demonstrate the potential of SLE to repair and manufacture single-crystal hot section components of gas turbine systems from nickel-based superalloy powders.

Unidirectional growth of benzil crystal from solution by Sankaranarayanan-Ramasamy method and its characterization

NASA Astrophysics Data System (ADS)

Rajalakshmi, M.; Shyju, T. S.; Indirajith, R.; Gopalakrishnan, R.

2012-02-01

Good quality <1 0 0> benzil single crystal with a diameter 18 mm and length 75 mm was successfully grown from solution by the unidirectional growth method of Sankaranarayanan-Ramasamy (SR) for the first time in the literature. The seed crystals have been harvested from conventional solution growth technique and subsequently used for unidirectional growth. The grown crystal was subjected to various characterization studies. The results of UV-vis spectral analysis, photoluminescence, etching and microhardness studies were compared with conventional solution grown crystal to that of SR method grown crystal. The quality of SR method grown benzil crystal is better than conventional solution grown crystal.

Crystal and Vibrational Structure of Energetic 3,5-dinitro 1,3,5-oxadiazinane (DOD) by Single Crystal X-ray Diffractometry and Raman Spectroscopy

DTIC Science & Technology

2018-03-19

calculations using a temperature of 298 K. 15. SUBJECT TERMS 3,5-dinitro-1,3,5-oxadiazinane (DOD), X-ray crystallography , Raman, energetic material...X-ray analysis. 2.2 Characterization X-ray Crystallography . DOD crystals were characterized with a SuperNova, Dualflex, EosS2 diffractometer using

Growth and characterization of Methyl 2-amino-5-bromobenzoate crystal for NLO applications

NASA Astrophysics Data System (ADS)

Parthasarathy, M.; Gopalakrishnan, R.

2012-11-01

Good quality single crystal of organic Methyl 2-amino-5-bromobenzoate (M2A5B) was grown using slow evaporation solution growth technique. The grown crystal was confirmed by single crystal X-ray diffraction. The functional groups and vibrational frequencies were identified using FT-IR and FT-Raman spectral analyses. The presence of hydrogen and carbon atoms in the grown sample was confirmed with proton and carbon NMR spectral studies. The optical energy band gap of the title compound is found to be 2.7 eV from the optical transmission spectra. The refractive indices nx, ny, and nz were found to be 1.569, 1.587 and 1.600, respectively using Brewster's angle method. The melting point of the material obtained with melting point apparatus is 74 °C. Thermal stability of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The mechanical behaviour of the grown crystal was analyzed with Vicker's microhardness tester. The particle size dependent second harmonic generation efficiency for M2A5B was evaluated by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching.

Defect studies of ZnO single crystals electrochemically doped with hydrogen

NASA Astrophysics Data System (ADS)

Čížek, J.; Žaludová, N.; Vlach, M.; Daniš, S.; Kuriplach, J.; Procházka, I.; Brauer, G.; Anwand, W.; Grambole, D.; Skorupa, W.; Gemma, R.; Kirchheim, R.; Pundt, A.

2008-03-01

Various defect studies of hydrothermally grown (0001) oriented ZnO crystals electrochemically doped with hydrogen are presented. The hydrogen content in the crystals is determined by nuclear reaction analysis and it is found that already 0.3at.% H exists in chemically bound form in the virgin ZnO crystals. A single positron lifetime of 182ps is detected in the virgin crystals and attributed to saturated positron trapping at Zn vacancies surrounded by hydrogen atoms. It is demonstrated that a very high amount of hydrogen (up to ˜30at.%) can be introduced into the crystals by electrochemical doping. More than half of this amount is chemically bound, i.e., incorporated into the ZnO crystal lattice. This drastic increase of the hydrogen concentration is of marginal impact on the measured positron lifetime, whereas a contribution of positrons annihilated by electrons belonging to O-H bonds formed in the hydrogen doped crystal is found in coincidence Doppler broadening spectra. The formation of hexagonal shape pyramids on the surface of the hydrogen doped crystals by optical microscopy is observed and discussed.

Synthesis and structural study of 4-(2-chlorophenyl)-2-ethoxy-5,6,7,8,9,10-hexahydrocycloocta[B] pyridine-3-carbonitrile

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fathima, K. Saiadali; Vasumathi, M.; Anitha, K., E-mail: singlecrystalxrd@gmail.com

2016-05-23

The novel organic material C{sub 20}H{sub 21}ClN{sub 2}O was synthesized by One-Pot synthesis method and the single crystals were grown by slow evaporation solution growth technique. The crystal structure was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R=0.039 for 2746 reflections. Crystal system of the grown crystal was found to be monoclinic with the space group P2{sub 1}/a and a=9.196(4) Å, b=13.449(4) Å, c=14.818(4) Å, β= 101.542(3)°, V=1795.6(11) Å{sup 3} and Z=4. In this crystal structure, cyclooctanone prefers to reside in a chair-boat conformation. Themore » structure is stabilized by attractive molecular force such as CH/π interaction called hydrophobic interaction.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Piyush, E-mail: piyush-patel130@yahoo.com; Vyas, S. M., E-mail: s-m-vyas-gu@hotmail.com; Patel, Vimal

The III-VI compound semiconductors is important for the fabrication of ionizing radiation detectors, solid-state electrodes, and photosensitive heterostructures, solar cell and ionic batteries. In this paper, In{sub 2}Se{sub 2.7} Sb{sub 0.3} single crystals were grown by the Bridgman method with temperature gradient of 60 °C/cm and the growth velocity 0.5cm/hr. The as-grown crystals were examined under the optical microscope for surface study, a various growth features observed on top free surface of the single crystal which is predominant of layers growth mechanism. The lattice parameters of as-grown crystal was determined by the XRD analysis. A Vickers’ projection microscope were usedmore » for the study of microhardness on the as-cleaved, cold-worked and annealed samples of the crystals, the results were discussed, and reported in detail.« less

Scintillation properties of Li6Y0.5Gd0.5(BO3)3: Ce3+ single crystal

NASA Astrophysics Data System (ADS)

Fawad, U.; Rooh, Gul; Kim, H. J.; Park, H.; Kim, Sunghwan; Khan, Sajid

2015-01-01

The Ce3+ doped mixed crystals of Li6Y(BO3)3 and Li6Gd(BO3)3 are grown by Czochralski technique with equal mole ratios of both Yttrium and Gadolinium i.e. Li6Y0.5Gd0.5(BO3)3. The grown crystals have the dimensions of ∅10×30 mm2. Powder X-ray diffraction (XRD) analysis confirmed single phase of the grown crystals. X-ray and laser induced luminescence spectra are presented. Scintillation properties such as energy resolution, light yield, decay time and α/β ratio under the excitation of 137Cs γ-ray photons and 241Am α-particles are also reported in this article.

An equivalent dipole analysis of PZT ceramics and lead-free piezoelectric single crystals

NASA Astrophysics Data System (ADS)

Bell, Andrew J.

2016-04-01

The recently proposed Equivalent Dipole Model for describing the electromechanical properties of ionic solids in terms of 3 ions and 2 bonds has been applied to PZT ceramics and lead-free single crystal piezoelectric materials, providing analysis in terms of an effective ionic charge and the asymmetry of the interatomic force constants. For PZT it is shown that, as a function of composition across the morphotropic phase boundary, the dominant bond compliance peaks at 52% ZrO2. The stiffer of the two bonds shows little composition dependence with no anomaly at the phase boundary. The effective charge has a maximum value at 50% ZrO2, decreasing across the phase boundary region, but becoming constant in the rhombohedral phase. The single crystals confirm that both the asymmetry in the force constants and the magnitude of effective charge are equally important in determining the values of the piezoelectric charge coefficient and the electromechanical coupling coefficient. Both are apparently temperature dependent, increasing markedly on approaching the Curie temperature.

Superconductivity and valence state in layered single-crystal HfAs1.67Te0.12

NASA Astrophysics Data System (ADS)

Peng, Jian; Yu, Jia; Zhang, Shuai; Chen, Genfu

2018-01-01

We report a detailed study on single crystals of HfAs1.67Te0.12 within a PbFCl-type layered structure. The single crystals of the title compound were successfully grown using a chemical transport reaction. The temperature dependence of electrical resistivity ρ (T), AC magnetic susceptibility {χ }{AC}(T) and specific heat C(T) show a bulk superconductivity with transition temperature T c = 1.67 K. The jump of C/T at T c is comparable to the traditional BCS weak-coupling model. A full H-T phase diagram is established using the results of ρ (T,H) and C(T) under fields, suggesting a rather weak anisotropy [({H}c2\\parallel {ab}(0)/{H}c2\\parallel c(0)] of 1.8 in orbital limit dominated three-dimension-like superconducting system. The mixed-valence states of Hf and As observed in the binding energy from x-ray photoelectron spectroscopy are consistent with the single-crystal x-ray diffraction analysis, indicating that the As-Te disorder prefers to occur in the [HfAs] layer and a large amount of vacancies are present in tetragonal As layer. As compared to HfAs1.7Se0.2 (T c = 0.52 K), a positive-like vacancy effect on T c has been confirmed in HfAs1.67Te0.12. The analysis of the Hall coefficient implies that the hole-type carriers dominate the transport properties, which is in good agreement with the hole pockets at Fermi surface obtained in a band structure calculation. The detailed study of single-crystal HfAs1.67Te0.12 provides a possible candidate to discuss the non-magnetic Kondo effect.

Combining EPR spectroscopy and X-ray crystallography to elucidate the structure and dynamics of conformationally constrained spin labels in T4 lysozyme single crystals.

PubMed

Consentius, Philipp; Gohlke, Ulrich; Loll, Bernhard; Alings, Claudia; Heinemann, Udo; Wahl, Markus C; Risse, Thomas

2017-08-09

Electron paramagnetic resonance (EPR) spectroscopy in combination with site-directed spin labeling is used to investigate the structure and dynamics of conformationally constrained spin labels in T4 lysozyme single crystals. Within a single crystal, the oriented ensemble of spin bearing moieties results in a strong angle dependence of the EPR spectra. A quantitative description of the EPR spectra requires the determination of the unit cell orientation with respect to the sample tube and the orientation of the spin bearing moieties within the crystal lattice. Angle dependent EPR spectra were analyzed by line shape simulations using the stochastic Liouville equation approach developed by Freed and co-workers and an effective Hamiltonian approach. The gain in spectral information obtained from the EPR spectra of single crystalline samples taken at different frequencies, namely the X-band and Q-band, allows us to discriminate between motional models describing the spectra of isotropic solutions similarly well. In addition, it is shown that the angle dependent single crystal spectra allow us to identify two spin label rotamers with very similar side chain dynamics. These results demonstrate the utility of single crystal EPR spectroscopy in combination with spectral line shape simulation techniques to extract valuable dynamic information not readily available from the analysis of isotropic systems. In addition, it will be shown that the loss of electron density in high resolution diffraction experiments at room temperature does not allow us to conclude that there is significant structural disorder in the system.

Generation of crystal structures using known crystal structures as analogues

PubMed Central

Cole, Jason C.; Groom, Colin R.; Read, Murray G.; Giangreco, Ilenia; McCabe, Patrick; Reilly, Anthony M.; Shields, Gregory P.

2016-01-01

This analysis attempts to answer the question of whether similar molecules crystallize in a similar manner. An analysis of structures in the Cambridge Structural Database shows that the answer is yes – sometimes they do, particularly for single-component structures. However, one does need to define what we mean by similar in both cases. Building on this observation we then demonstrate how this correlation between shape similarity and packing similarity can be used to generate potential lattices for molecules with no known crystal structure. Simple intermolecular interaction potentials can be used to minimize these potential lattices. Finally we discuss the many limitations of this approach. PMID:27484374

Stabilization of Quinapril by Incorporating Hydrogen Bonding Interactions

PubMed Central

Roy, B. N.; Singh, G. P.; Godbole, H. M.; Nehate, S. P.

2009-01-01

In the present study stability of various known solvates of quinapril hydrochloride has been compared with nitromethane solvate. Nitromethane solvate was found to be more stable compared to other known solvates. Single crystal X-ray diffraction analysis of quinapril nitromethane solvate shows intermolecular hydrogen bonding between quinapril molecule and nitromethane. Stabilization of quinapril by forming strong hydrogen bonding network as in case of co-crystals was further studied by forming co-crystal with tris(hydroxymethyl)amino methane. Quinapril free base forms a stable salt with tris(hydroxymethyl)amino methane not reported earlier. Quinapril tris(hydroxymethyl)amino methane salt found to be stable even at 80° for 72 h i.e. hardly any formation of diketopiperazine and diacid impurity. As expected single crystal X-ray diffraction analysis reveals tris(hydroxymethyl)amino methane salt of quinapril shows complex hydrogen bonding network between the two entities along with ionic bond. The properties of this stable salt - stable in solid as well as solution phase, might lead to an alternate highly stable formulation. PMID:20502545

New investigations of the guanine trichloro cuprate(II) complex crystal

NASA Astrophysics Data System (ADS)

Fabijanić, Ivana; Matković-Čalogović, Dubravka; Pilepić, Viktor; Ivanišević, Irena; Mohaček-Grošev, Vlasta; Sanković, Krešimir

2017-01-01

Crystals of the guanine trichloro cuprate(II) complex, (HGua)2[Cu2Cl6]·2H2O (HGua = protonated guanine), were prepared and analysed by spectroscopic (IR, Raman) and computational methods. A new single-crystal X-ray diffraction analysis was conducted to obtain data with lower standard uncertainties than those in the previously published structure. Raman and IR spectroscopy and quantum-mechanical analysis gave us new insight into the vibrational states of the (HGua)2[Cu2Cl6]·2H2O crystal. The vibrational spectra of the crystal were assigned by performing a normal coordinate analysis for a free dimer with a centre of inversion as the only symmetry element. The stretching vibration observed at 279 cm-1 in the infrared spectrum corresponds to the N-Cu bond. The noncovalent interaction (NCI) plots and quantum theory of atoms in molecules (QTAIM) analysis of the electron density obtained from periodic DFT calculations elucidated the interactions that exist within the crystal structure. Closed-shell ionic attractions, as well as weak and medium strength hydrogen bonds, prevailed in the crystal packing.

Synthesis, growth, structural, optical, spectral, thermal and mechanical studies of 4-methoxy 4-nitrostilbene (MONS): a new organic nonlinear optical single crystal.

PubMed

Dinakaran, Paul M; Bhagavannarayana, G; Kalainathan, S

2012-11-01

4-Methoxy 4-nitrostilbene (MONS), a new organic nonlinear optical material has been synthesized. Based on the solubility data good quality single crystal with dimensions up to 38×11×3 mm(3) has been grown by slow evaporation method using ethyl methyl ketone (MEK) as a solvent. Powder XRD confirms the crystalline property and also the diffraction planes have been indexed. The lattice parameters for the grown MONS crystals were determined by using single crystal X-ray diffraction analysis and it reveals that the crystal lattice system is triclinic. The crystalline perfection of the grown crystals has been analysed by high resolution X-ray diffraction (HRXRD) rocking curve measurements. Fourier transform infrared (FTIR) spectrum for powdered MONS sample confirms the functional groups present in the grown crystal. The UV-vis absorption spectrum has been recorded in the range of 190-1100 nm and the cut off wavelength 499 nm has been determined. The optical constants of MONS have been determined through UV-vis-NIR spectroscopy. The MONS crystals were further subjected to other characterizations. i.e., (1)H NMR, TG/DTA, photoluminescence and microhardness test. The Kurtz and Perry powder technique confirms the NLO property of the grown crystal and the SHG efficiency of MONS was found to be 1.55× greater than that of KDP crystal. Copyright © 2012 Elsevier B.V. All rights reserved.

LCP crystallization and X-ray diffraction analysis of VcmN, a MATE transporter from Vibrio cholerae

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kusakizako, Tsukasa; Tanaka, Yoshiki; Hipolito, Christopher J.

A V. cholerae MATE transporter was crystallized using the lipidic cubic phase (LCP) method. X-ray diffraction data sets were collected from single crystals obtained in a sandwich plate and a sitting-drop plate to resolutions of 2.5 and 2.2 Å, respectively. Multidrug and toxic compound extrusion (MATE) transporters, one of the multidrug exporter families, efflux xenobiotics towards the extracellular side of the membrane. Since MATE transporters expressed in bacterial pathogens contribute to multidrug resistance, they are important therapeutic targets. Here, a MATE-transporter homologue from Vibrio cholerae, VcmN, was overexpressed in Escherichia coli, purified and crystallized in lipidic cubic phase (LCP). X-raymore » diffraction data were collected to 2.5 Å resolution from a single crystal obtained in a sandwich plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 52.3, b = 93.7, c = 100.2 Å. As a result of further LCP crystallization trials, crystals of larger size were obtained using sitting-drop plates. X-ray diffraction data were collected to 2.2 Å resolution from a single crystal obtained in a sitting-drop plate. The crystal belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 61.9, b = 91.8, c = 100.9 Å. The present work provides valuable insights into the atomic resolution structure determination of membrane transporters.« less

HRTEM Analysis of Crystallographic Defects in CdZnTe Single Crystal

NASA Astrophysics Data System (ADS)

Yasar, Bengisu; Ergunt, Yasin; Kabukcuoglu, Merve Pinar; Parlak, Mehmet; Turan, Rasit; Kalay, Yunus Eren

2018-01-01

In recent years, CdZnTe has attracted much attention due to its superior electrical and structural properties for room-temperature operable gamma and x-ray detectors. However, CdZnTe (CZT) material has often suffered from crystallographic defects encountered during the growth and post-growth processes. The identification and structural characterization of these defects is crucial to synthesize defect-free CdZnTe single crystals. In this study, Cd0.95 Zn0.05 Te single crystals were grown using a three-zone vertical Bridgman system. The single crystallinity of the material was ensured by using x-ray diffraction measurements. High-resolution electron microscopy (HRTEM) was used to characterize the nano-scale defects on the CdZnTe matrix. The linear defects oriented along the ⟨211⟩ direction were examined by transmission electron microscopy (TEM) and the corresponding HRTEM image simulations were performed by using a quantitative scanning TEM simulation package.

Efficiency of different methods of extra-cavity second harmonic generation of continuous wave single-frequency radiation.

PubMed

Khripunov, Sergey; Kobtsev, Sergey; Radnatarov, Daba

2016-01-20

This work presents for the first time to the best of our knowledge a comparative efficiency analysis among various techniques of extra-cavity second harmonic generation (SHG) of continuous-wave single-frequency radiation in nonperiodically poled nonlinear crystals within a broad range of power levels. Efficiency of nonlinear radiation transformation at powers from 1 W to 10 kW was studied in three different configurations: with an external power-enhancement cavity and without the cavity in the case of single and double radiation pass through a nonlinear crystal. It is demonstrated that at power levels exceeding 1 kW, the efficiencies of methods with and without external power-enhancement cavities become comparable, whereas at even higher powers, SHG by a single or double pass through a nonlinear crystal becomes preferable because of the relatively high efficiency of nonlinear transformation and fairly simple implementation.

Sponge-like nanoporous single crystals of gold

PubMed Central

Khristosov, Maria Koifman; Bloch, Leonid; Burghammer, Manfred; Kauffmann, Yaron; Katsman, Alex; Pokroy, Boaz

2015-01-01

Single crystals in nature often demonstrate fascinating intricate porous morphologies rather than classical faceted surfaces. We attempt to grow such crystals, drawing inspiration from biogenic porous single crystals. Here we show that nanoporous single crystals of gold can be grown with no need for any elaborate fabrication steps. These crystals are found to grow following solidification of a eutectic composition melt that forms as a result of the dewetting of nanometric thin films. We also present a kinetic model that shows how this nano-porous single-crystalline structure can be obtained, and which allows the potential size of the porous single crystal to be predicted. Retaining their single-crystalline nature is due to the fact that the full crystallization process is faster than the average period between two subsequent nucleation events. Our findings clearly demonstrate that it is possible to form single-crystalline nano porous metal crystals in a controlled manner. PMID:26554856

Growth, nonlinear optical, thermal, dielectric and laser damage threshold studies of semiorganic crystal: monohydrate piperazine hydrogen phosphate.

PubMed

Krishnan, P; Gayathri, K; Bhagavannarayana, G; Gunasekaran, S; Anbalagan, G

2013-02-01

Monohydrate piperazine hydrogen phosphate (MPHP), a semi organic nonlinear optical material has been synthesized and single crystals were grown from aqueous solution by slow evaporation technique. Single crystal X-ray diffraction study on grown crystal reveals that they belong to monoclinic crystal system with space group P2(1)/c; (a=6.39Å; b=12.22Å; c=11.16Å; β=97.14°; V=864Å(3)). The structural perfection of the grown crystal was analyzed by high-resolution X-ray diffraction (HRXRD) rocking curve measurements. FTIR spectrum confirms the presence of the functional groups in synthesized material. UV-Vis spectrum indicates that the crystal is transparent in the entire visible region with a lower cut off wavelength of 387 nm. The variation of dielectric properties of the grown crystal with respect to frequency has been investigated at different temperatures. Thermal analysis carried out on the MPHP crystal shows that the crystal is stable up to 135°C. Relative powder second harmonic generation efficiency tested by Kurtz-Perry powder technique, which was about 0.638 times that of Potassium dihydrogen phosphate. Copyright © 2012 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yu; Petrovic, C.

CrI 3 is a promising candidate for the van der Waals bonded ferromagnetic devices since its ferromagnetism can be maintained upon exfoliating of bulk crystals down to single layer. In this work we studied critical properties of bulk CrI 3 single crystals around the paramagnetic to ferromagnetic phase transition. Critical exponents β= 0.260(4) with a critical temperature T c= 60.05(13) K and γ= 1.136(6) with T c= 60.43(4) K are obtained by the Kouvel-Fisher method, whereas δ= 5.32(2) is obtained by a critical isotherm analysis at T c= 60 K. In conclusion, the critical exponents determined in bulk CrI 3more » single crystals suggest a three-dimensional long-range magnetic coupling with the exchange distance decaying as J(r)≈r -4:69« less

Structural and electronic evolution of Cr[subscript 2]O[subscript 3] on compression to 55 GPa

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dera, Przemyslaw; Lavina, Barbara; Meng, Yue

2016-08-15

Synchrotron single-crystal x-ray diffraction experiments have been performed on corundum-type Cr{sub 2}O{sub 3} up to a pressure of 55 GPa in Ne and He pressure transmitting media. Diffraction experiments were complemented by measurements of optical absorption spectra with single crystal samples up to 60 GPa. Results of the diffraction data analysis rule out the earlier reported monoclinic distortion at 15-30 GPa, but indicate evidence of two discontinuous transitions of electronic or magnetic nature, most likely associated with a change in magnetic ordering and charge transfer. The compression mechanism established from single crystal refinements indicates much smaller distortion of the Cr{supmore » 3+} coordination environment than was previously assumed.« less

Single-crystal growth, structure refinement and the properties of Bis(glycine) Strontium Chloride

NASA Astrophysics Data System (ADS)

Balaji, S. R.; Balu, T.; Rajasekaran, T. R.

2018-02-01

Single crystals of Bis (glycine) Strontium Chloride (BGSC) were grown by means of slow evaporation process by using analar grade Glycine and Strontium Chloride Hexahydrate as a parent compound from its aqueous solution at room temperature. The final chemical composition, [{{Sr}}{({{{C}}}2{{{H}}}5{{{NO}}}2)}2{{{Cl}}}2].{{{H}}}4{{{O}}}3+{{{H}}}8{{{O}}}3, formed were metallic light colorless block, about the size of 28 mm × 9 mm × 8 mm. A single-crystal x-ray diffraction study revealed an ordered superstructure with orthorhombic symmetry that could be assigned to the space group Pbcn. The structure in BGSC, revealed in the electron density distribution was analyzed by the direct methods (SHELXS-2014) and refined by least squares full matrix method (SHELXL-2014). The crystal structure, including anisotropic atomic displacement parameters for each atom and isotropic atomic displacement parameters for hydrogen atom, was refined to R1 = 0.0395, wR2 = 0.0776 using 1097 independent reflections. The FTIR spectrum of BGSC confirms the protonation of amino groups and the different molecular groups present in BGSC vibrate in different modes. Reverse Indentation Size Effect (RISE) was revealed in BGSC in the micro-hardness analysis using Vicker’s micro-hardness analysis. DTA and DSC results ruled out the possibility of structural change independent of mass change. The AFM studies shows fine nano size fiber like structure of the grown crystals.

Crystal growth and characterization of the CMR compound La 1.2(Sr,Ca) 1.8Mn 2O 7

NASA Astrophysics Data System (ADS)

Velázquez, M.; Haut, C.; Hennion, B.; Revcolevschi, A.

2000-12-01

High-quality centimeter-sized single crystals of La 1.2Sr 1.8- yCa yMn 2O 7 (0.0⩽ y⩽0.2) were successfully grown using a floating zone method associated with an image furnace. We present the growth conditions together with a characterization of the single crystals by means of optical and electron microscopy, EDX and ICP⧸AES analysis, DTA-TGA measurements and redox titration, X-ray powder diffraction, Laue X-ray back-reflection and neutron diffraction. We also stress the main aspects of the complex thermodynamical and kinetic behaviors of these compounds.

Dosimetry with diamond detectors

NASA Astrophysics Data System (ADS)

Gervino, G.; Marino, C.; Silvestri, F.; Lavagno, A.; Truc, F.

2010-05-01

In this paper we present the dosimetry analysis in terms of stability and repeatability of the signal and dose rate dependence of a synthetic single crystal diamond grown by Chemical Vapor Deposition (CVD) technique. The measurements carried out by 5 MeV X-ray photons beam show very promising results, even if the dose rate detector response points out that the charge trapping centers distribution is not uniform inside the crystal volume. This handicap that affects the detectors performances, must be ascribed to the growing process. Synthetic single crystal diamonds could be a valuable alternative to air ionization chambers for quality beam control and for intensity modulated radiation therapy beams dosimetry.

Atomic Migration Induced Crystal Structure Transformation and Core-Centered Phase Transition in Single Crystal Ge2Sb2Te5 Nanowires.

PubMed

Lee, Jun-Young; Kim, Jeong-Hyeon; Jeon, Deok-Jin; Han, Jaehyun; Yeo, Jong-Souk

2016-10-12

A phase change nanowire holds a promise for nonvolatile memory applications, but its transition mechanism has remained unclear due to the analytical difficulties at atomic resolution. Here we obtain a deeper understanding on the phase transition of a single crystalline Ge 2 Sb 2 Te 5 nanowire (GST NW) using atomic scale imaging, diffraction, and chemical analysis. Our cross-sectional analysis has shown that the as-grown hexagonal close-packed structure of the single crystal GST NW transforms to a metastable face-centered cubic structure due to the atomic migration to the pre-existing vacancy layers in the hcp structure going through iterative electrical switching. We call this crystal structure transformation "metastabilization", which is also confirmed by the increase of set-resistance during the switching operation. For the set to reset transition between crystalline and amorphous phases, high-resolution imaging indicates that the longitudinal center of the nanowire mainly undergoes phase transition. According to the atomic scale analysis of the GST NW after repeated electrical switching, partial crystallites are distributed around the core-centered amorphous region of the nanowire where atomic migration is mainly induced, thus potentially leading to low power electrical switching. These results provide a novel understanding of phase change nanowires, and can be applied to enhance the design of nanowire phase change memory devices for improved electrical performance.

A new cadmium(II) complex with bridging dithiolate ligand: Synthesis, crystal structure and antifungal activity study

NASA Astrophysics Data System (ADS)

Singh, Mahesh Kumar; Sutradhar, Sanjit; Paul, Bijaya; Adhikari, Suman; Laskar, Folguni; Butcher, Raymond J.; Acharya, Sandeep; Das, Arijit

2017-07-01

A new polymeric complex of Cd(II) with 1,1-dicyanoethylene- 2,2-dithiolate [ i-MNT2- = {S2C:C(CN)2}2- ] as a bridging ligand has been synthesized and characterized on the basis of spectroscopy and single-crystal X-ray diffraction analysis. Single crystal X-ray diffraction analysis reveals that the Cadmium (II) complex is six coordinated 1D polymeric in nature. Biological screening effects in vitro of the synthesized polymeric complex has been tested against five fungi Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans(ATCC10231), Trichophyton mentagrophytes by the disc diffusion method. In vitro antifungal screening indicates that the complex exhibits fungistatic and fungicidal antifungal activity whereas K2i-MNT.H2O became silent on Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans (ATCC10231), Trichophyton mentagrophytes.

Detailed Surface Analysis Of Incremental Centrifugal Barrel Polishing (CBP) Of Single-Crystal Niobium Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Palczewski, Ari D.; Tian, Hui; Trofimova, Olga

2011-07-01

We performed Centrifugal Barrel Polishing (CBP) on single crystal niobium samples/coupons housed in a stainless steel sample holder following the polishing recipe developed at Fermi Lab (FNAL) in 2011 \\cite{C. A. Cooper 2011}. Post CBP, the sample coupons were analyzed for surface roughness, crystal composition and structure, and particle contamination. Following the initial analysis each coupon was high pressure rinsed (HRP) and analyzed for the effectiveness of contamination removal. We were able to obtain the mirror like surface finish after the final stage of tumbling, although some defects and embedded particles remained. In addition, standard HPR appears to have littlemore » effect on removing embedded particles which remain after each tumbling step, although final polishing media removal was partially affected by standard/extended HPR.« less

Surface force analysis of glycine adsorption on different crystal surfaces of titanium dioxide (TiO2).

PubMed

Ganbaatar, Narangerel; Imai, Kanae; Yano, Taka-Aki; Hara, Masahiko

2017-01-01

Surface force analysis with atomic force microscope (AFM) in which a single amino acid residue was mounted on the tip apex of AFM probe was carried out for the first time at the molecular level on titanium dioxide (TiO 2 ) as a representative mineral surface for prebiotic chemical evolution reactions. The force analyses on surfaces with three different crystal orientations revealed that the TiO 2 (110) surface has unique characteristics for adsorbing glycine molecules showing different features compared to those on TiO 2 (001) and (100). To examine this difference, we investigated thermal desorption spectroscopy (TDS) and the interaction between the PEG cross-linker and the three TiO 2 surfaces. Our data suggest that the different single crystal surfaces would provide different chemical evolution field for amino acid molecules.

Single crystal X-ray diffraction study of the HgBa2CuO4+δ superconducting compound

NASA Astrophysics Data System (ADS)

Bordet, P.; Duc, F.; Lefloch, S.; Capponi, J. J.; Alexandre, E.; Rosa-Nunes, M.; Antipov, E. V.; Putilin, S.

1996-02-01

A high precision X-ray diffraction analysis up to sin θ/λ = 1.15 of a HgBa2CuO4+δ single crystal having a Tc of ~ 90 K is presented. The cell parameters are a = 3.8815(4), c = 9.485 (7) Å. The refinements indicate the existence of a split barium site due to the presence of excess oxygen in the mercury layer. The position of this excess oxygen might be slightly displaced from the (1/2 1/2 0) position. A 6% mercury deficiency is observed. Models, including mercury defects, substitution by copper cations, or carbonate groups, are compared. However, we obtain no definite evidence for either of the three models. A possible disorder of the Hg position, due to the formation of chemical bonds with neighbouring extra oxygen anions, could correlate to the refinements of mixed species at the Hg site. A low temperature single crystal x-ray diffraction study, and comparison of refinements for the same single crystal with different extra oxygen contents, are in progress to help clarify this problem.

Fluorescence X-ray absorption spectroscopy using a Ge pixel array detector: application to high-temperature superconducting thin-film single crystals.

PubMed

Oyanagi, H; Tsukada, A; Naito, M; Saini, N L; Lampert, M O; Gutknecht, D; Dressler, P; Ogawa, S; Kasai, K; Mohamed, S; Fukano, A

2006-07-01

A Ge pixel array detector with 100 segments was applied to fluorescence X-ray absorption spectroscopy, probing the local structure of high-temperature superconducting thin-film single crystals (100 nm in thickness). Independent monitoring of pixel signals allows real-time inspection of artifacts owing to substrate diffractions. By optimizing the grazing-incidence angle theta and adjusting the azimuthal angle phi, smooth extended X-ray absorption fine structure (EXAFS) oscillations were obtained for strained (La,Sr)2CuO4 thin-film single crystals grown by molecular beam epitaxy. The results of EXAFS data analysis show that the local structure (CuO6 octahedron) in (La,Sr)2CuO4 thin films grown on LaSrAlO4 and SrTiO3 substrates is uniaxially distorted changing the tetragonality by approximately 5 x 10(-3) in accordance with the crystallographic lattice mismatch. It is demonstrated that the local structure of thin-film single crystals can be probed with high accuracy at low temperature without interference from substrates.

High-quality single-crystal thulium iron garnet films with perpendicular magnetic anisotropy by off-axis sputtering

NASA Astrophysics Data System (ADS)

Wu, C. N.; Tseng, C. C.; Lin, K. Y.; Cheng, C. K.; Yeh, S. L.; Fanchiang, Y. T.; Hong, M.; Kwo, J.

2018-05-01

High-quality single-crystal thulium iron garnet (TmIG) films of 10-30 nm thick were grown by off-axis sputtering at room temperature (RT) followed by post-annealing. X-ray photoelectron spectroscopy (XPS) was employed to determine the TmIG film composition to optimize the growth conditions, along with the aid of x-ray diffraction (XRD) structural analysis and atomic force microscope (AFM) for surface morphology. The optimized films exhibited perpendicular magnetic anisotropy (PMA) and the saturation magnetization at RT was ˜99 emu/cm3, close to the RT bulk value ˜110 emu/cm3 with a very low coercive field of ˜2.4 Oe. We extracted the H⊥ of 1734 Oe and the peak-to-peak linewidth ΔH of ferromagnetic resonance are only about 99 Oe, significantly lower than that of PLD grown TmIG film and bulk single crystals. The high-quality sputtered single-crystal TmIG films show great potential to be integrated with topological insulators or heavy metals with strong spin-orbit coupling for spintronic applications.

Work-hardening behaviour of Mg single crystals oriented for basal slip

NASA Astrophysics Data System (ADS)

Bhattacharya, B.; Niewczas, M.

2011-06-01

Work-hardening behaviour of Mg single crystals oriented for basal slip was studied by means of tensile tests carried out at 4, 78 and 295 K. The crystals show critical resolved shear stress values (CRSS) for a {0001} ? basal slip system in the range 1-1.5 MPa. The samples exhibit two-stage work hardening characteristics consisting of a long easy glide stage and a stage of rapid hardening terminated by failure. The onset of the plastic flow up to the point of fracture is accompanied by a low work-hardening rate in the range 5 × 10-5-5 × 10-4 µ, corresponding to the hardening rate in Stage I of copper single crystals. The analysis of thermally activated glide parameters suggests that forest interactions are rate-controlling processes. The very low value of the activation distance found at 4 K, ∼0.047 b, is attributed to zero-point energy effects. The failure of crystals occurs well before their hardening capacity is exhausted by mechanisms which are characteristic of deformation temperature.

Analysis of spin-Hamiltonian and molecular orbital coefficients of Cu2+ doped C8H11KO8 single crystal through EPR technique

NASA Astrophysics Data System (ADS)

Juliet sheela, K.; Krishnan, S. Radha; Shanmugam, V. M.; Subramanian, P.

2018-04-01

Electron paramagnetic resonance (EPR) studies have been investigated at X-band microwave frequency on Cu2+ ion incorporated into the single crystal of potassium succinate-succinic acid (KSSA) at room temperature. The angular variation of the EPR spectra has shown two magnetically in-equivalent Cu2+ sites in the KSSA single crystal system. The spin Hamiltonian parameters g and A are determined which reveals that the site I and site II occupied in rhombic and axial local field symmetry around the impurity ion. Among the two paramagnetic impurity ions, sites one occupies at substituitional position in the place of monovalent cation (K+) in the crystal whereas the other enters in its lattice interstitially by the correlation of EPR and crystal structure data. From the calculated principle values gxx, gyy, gzz and Axx, Ayy, Azz of both the sites, the admixture coefficients and molecular orbital coefficients were evaluated which gives the information of ground state wave function and types of bonding of impurity ions with the ligands.

Structural, vibrational, thermal and optical studies of organic single crystal: Benzotriazolium p-toluene sulfonate (BTPTS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, R. Ramesh; Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@yahoo.com

Benzotriazolium p-toluene sulfonate (BTPTS) was grown by solution growth technique. The powder X-ray diffraction analysis was carried out to evaluate crystal system of the compound. LeBail Profile fitting analysis was performed to extract the individual peak intensities. FTIR spectrum analysis was recorded to study vibration frequencies of the prepared organic salt. Thermal studies were carried out using TG-DSC analysis. Optical absorption and energy band gap of the title compound was evaluated by UV-Vis spectral study.

Unidirectional growth of benzil crystal from solution by Sankaranarayanan-Ramasamy method and its characterization.

PubMed

Rajalakshmi, M; Shyju, T S; Indirajith, R; Gopalakrishnan, R

2012-02-01

Good quality <100> benzil single crystal with a diameter 18 mm and length 75 mm was successfully grown from solution by the unidirectional growth method of Sankaranarayanan-Ramasamy (SR) for the first time in the literature. The seed crystals have been harvested from conventional solution growth technique and subsequently used for unidirectional growth. The grown crystal was subjected to various characterization studies. The results of UV-vis spectral analysis, photoluminescence, etching and microhardness studies were compared with conventional solution grown crystal to that of SR method grown crystal. The quality of SR method grown benzil crystal is better than conventional solution grown crystal. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis aspects, structural, spectroscopic, antimicrobial and room temperature ferromagnetism of zinc iodide complex with Schiff based ligand

NASA Astrophysics Data System (ADS)

Shakila, K.; Kalainathan, S.

2015-01-01

In this paper, we report the successful growth of complex compound of zinc iodide with thiocarbamide by slow evaporation method. The single crystal XRD study reveals that the crystal belongs to monoclinic system with centrosymmetric space group and powder XRD analysis shows that the perfect crystalline nature of the crystal. The presence of functional group and element were confirmed from FT-IR and EDAX analysis. Optical absorbance of the grown crystal was studied by UV-Vis spectrophotometer. The optical constants were calculated from the optical absorbance data such as refractive index (n), extinction coefficient (K) and reflectance (R). The optical band gap (Eg) of thiocarbamide zinc iodide crystal is 4.22 eV. The magnetic properties of grown crystal have been determined by Vibrating Sample Magnetometry (VSM). Room temperature magnetization revealed a ferromagnetic behaviour for the grown crystal. The antibacterial and antifungal activities of the title compound were performed by well diffusion method and MIC method against the standard bacteria like Staphylococcus aureus, Escherichia coli, Klebsiella pneumonia and against fungus like Aspergillus niger, Rhizopus sps and Penicillium sps. Thermal behaviour of the crystal has been investigated using thermogravimetric analysis (TGA) and differential thermal analysis (DTA).

Absolute configuration and crystal packing for three chiral drugs prone to spontaneous resolution: Guaifenesin, methocarbamol and mephenesin

NASA Astrophysics Data System (ADS)

Bredikhin, Alexander A.; Gubaidullin, Aidar T.; Bredikhina, Zemfira A.; Krivolapov, Dmitry B.; Pashagin, Alexander V.; Litvinov, Igor A.

2009-02-01

Popular chiral drugs, guaifenesin, methocarbamol, and mephenesin were investigated by single-crystal X-ray analysis both for enantiopure and racemic samples. The absolute configurations for all substances were established through Flack parameter method. The conglomerate-forming nature for the compounds was confirmed by equivalence of crystal characteristics of enantiopure and racemic samples. The molecular structures and crystal packing details were evaluated and compared with one another for all three investigated substances.

Aqueous Sulfate Separation by Sequestration of [(SO 4) 2(H 2O) 4] 4 Clusters within Highly Insoluble Imine-Linked Bis-Guanidinium Crystals

DOE PAGES

Custelcean, Radu; Williams, Neil J.; Seipp, Charles A.; ...

2015-12-18

Quantitative removal of sulfate from seawater was achieved by selective crystallization of the anion with a bis(guanidinium) ligand self-assembled in situ through imine condensation of simple components. The resulting crystalline salt has an exceptionally low aqueous solubility, on a par with BaSO 4. Single-crystal X-ray diffraction analysis revealed pairs of sulfate anions clustered together with four water molecules within the crystals.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sathyalakshmi, R.; Bhagavannarayana, G.; Ramasamy, P.

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 spectralmore » 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.« less

Conformational dimorphism of isochroman-1-ones in the solid state

NASA Astrophysics Data System (ADS)

Babjaková, Eva; Hanulíková, Barbora; Dastychová, Lenka; Kuřitka, Ivo; Nečas, Marek; Vícha, Robert

2014-12-01

Isochroman-1-one derivatives, which are relatives of coumarins, display a broad spectrum of biological activity; therefore, these derivatives attract the attention of chemists. A series of new isochroman-1-ones were prepared by the reaction of benzyl-derived Grignard reagents with acyl chlorides. All of the prepared compounds were characterized using single-crystal X-ray diffraction as well as FT-IR, NMR and MS techniques. Single crystal X-ray diffraction analysis revealed that the isochromanones can adopt two distinct conformations in the solid state. For one of the compounds, two polymorphs with unique forms crystallized separately under different temperatures. The packing of all of the examined crystals is stabilized via weak intramolecular C-H⋯π and/or C-H⋯O interactions. Although the closed conformer was predominantly found in the actual crystals, the open conformer is thermochemically more stable for all of the examined compounds according to DFT calculations.

Simplifying the growth of hybrid single-crystals by using nanoparticle precursors: the case of AgI

NASA Astrophysics Data System (ADS)

Xu, Biao; Wang, Ruji; Wang, Xun

2012-03-01

We report the synthesis of a series of AAgmIn single-crystals within 24 h, at room temperature, utilizing AgI nanoparticles (NPs) as the precursor. The AgI NPs impart high reactivity under mild conditions and favor the growth kinetics. 0D, 1D and 2D iodoargentate crystals can be obtained. This work represents the first application of NPs in the field of organo-metal-halide crystals and will inspire the design of other AMmXn crystals.We report the synthesis of a series of AAgmIn single-crystals within 24 h, at room temperature, utilizing AgI nanoparticles (NPs) as the precursor. The AgI NPs impart high reactivity under mild conditions and favor the growth kinetics. 0D, 1D and 2D iodoargentate crystals can be obtained. This work represents the first application of NPs in the field of organo-metal-halide crystals and will inspire the design of other AMmXn crystals. Electronic supplementary information (ESI) available: XPS spectra of AgI NPs, schematic representation of the formation process of [Ag4I8]4- in 2, UV-Vis spectra of the DTMA-Ag-I clusters, analysis of force balance of a crystal at the interface between H2O and CH2Cl2 and crystal structure depiction of 1-4. CIF files of 1-4 are also provided. CCDC reference numbers 863848, 863849, 863850 and 863851. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c2nr30139c

Luminescence and radiation resistance of undoped NaI crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shiran, N., E-mail: shiran@isc.kharkov.com; Boiaryntseva, I.; Gektin, A.

2014-11-15

Highlights: • The performance of NaI scintillators depends on luminescence properties. • A criterion of crystals’ purity level is radiation colorability at room temperature. • The traces of the most dangerous impurities were detected. • Crucial role in efficiency of pure NaI scintillator play the crystal perfection. - Abstract: Undoped NaI single crystal is an excellent scintillator at low temperature. However, scintillation parameters of different quality crystals vary in a wide range, significantly exceeding measurement error. Experimental data demonstrate the features of luminescence, radiation induced coloration, and afterglow dependence on the quality of nominally pure crystals. It is found thatmore » defects level that allows to elucidate artefacts introduced by traces of harmful impurities corresponds to 3 × 10{sup 15} cm{sup −3} that significantly overhead accuracy of chemical and absorption analysis. It is shown that special raw material treatment before and during the single crystal growth allows to reach NaI purity level that avoids impurities influence to the basic luminescence data.« less

Structural, optical, thermal and mechanical properties of Urea tartaric acid single crystals.

PubMed

Vinothkumar, P; Rajeswari, K; Kumar, R Mohan; Bhaskaran, A

2015-06-15

Urea tartaric acid (UT) an organic nonlinear optical (NLO) material was synthesized from aqueous solution and the crystals were grown by the slow evaporation technique. The single crystal X-ray diffraction (XRD) analysis revealed that the UT crystal belongs to the orthorhombic system. The functional groups of UT have been identified by the Fourier transform infrared spectral studies. The optical transparent window in the visible and near the IR regions was investigated. The transmittance of UT has been used to calculate the refractive index (n) as a function of the wavelength. The nonlinear optical property of the grown crystal has been confirmed by the Kurtz powder second harmonic generation test. The birefringence of the crystal was determined using a tungsten halogen lamp source. The laser induced surface damage threshold for the grown crystal was measured using the Nd:YAG laser. The anisotropic in mechanical property of the grown crystals was studied using Vicker's microhardness tester at different planes. The etch pit density of UT crystals was investigated. The thermal behavior of UT was investigated using the TG-DTA and DSC studies. Copyright © 2015 Elsevier B.V. All rights reserved.

Temperature induced phase transformations and negative electrocaloric effect in (Pb,La)(Zr,Sn,Ti)O3 antiferroelectric single crystal

NASA Astrophysics Data System (ADS)

Zhuo, Fangping; Li, Qiang; Yan, Qingfeng; Zhang, Yiling; Wu, Hong-Hui; Xi, Xiaoqing; Chu, Xiangcheng; Cao, Wenwu

2017-10-01

Temperature induced phase transitions and electrocaloric effect (ECE) of (Pb,La)(Zr,Sn,Ti)O3 (PLZST) single crystals have been comprehensively studied. Based on the in situ evolution of domain structures and dielectric properties of the PLZST crystals, the phase transitions during heating are in the sequence of orthorhombic antiferroelectric → rhombohedral ferroelectric → cubic paraelectric. Coexistence of the negative and positive ECEs has been achieved in the PLZST single crystals. A negative ECE value of -1.26 °C and enhanced electrocaloric strength of -0.21 K mm/kV near the Curie temperature have been obtained. A modified Landau model gives a satisfactory description of the experimentally observed unusual ECE. Moreover, a temperature-electric field phase diagram is also established based on theoretical analysis. Our results will help people understand better the electrocaloric family, particularly on the negative and/or positive effect in antiferroelectrics and ferroelectrics.

Silver transfer in proustite Ag{sub 3}AsS{sub 3} at high temperatures: Conductivity and single-crystal X-ray studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gagor, Anna; Pawlowski, Antoni; Pietraszko, Adam

2009-03-15

Single crystals of proustite Ag{sub 3}AsS{sub 3} have been characterised by impedance spectroscopy and single-crystal X-ray diffraction in the temperature ranges of 295-543 and 295-695 K, respectively. An analysis of the one-particle potential of silver atoms shows that in the whole measuring temperature range defects in the silver substructure play a major role in the conduction mechanism. Furthermore, the silver transfer is equally probable within silver chains and spirals, as well as between chains and spirals. The trigonal R3c room temperature phase does not change until the decomposition of the crystal. The electric anomaly of the first-order character which appearsmore » near 502 K is related to an increase in the electronic component of the total conductivity resulting from Ag{sub 2}S deposition at the sample surface. - Joint probability density function map of silver atoms at T=695 K.« less

Domain characterization of Pb(Zn1/3Nb2/3)O3-(6%-7%)PbTiO3 single crystals using scanning electron acoustic microscopy

NASA Astrophysics Data System (ADS)

Wong, Meng Fei; Heng, Xiangxin; Zeng, Kaiyang

2008-10-01

Domain structures of [001]T and [011]T-cut Pb(Zn1/3Nb2/3)O3-(6%-7%)PbTiO3 (PZN-PT) single crystals are studied using scanning electron acoustic microscope (SEAM) technique. The observation of the orientation of domain walls agree reasonably well with the trigonometric projection of rhombohedral and orthorhombic dipoles on the (001) and (011) surfaces, respectively. After mechanical loading with microindentation, domain switching is also observed to form a hyperbolic butterfly shape and extend preferentially along four diagonal directions, i.e., ⟨110⟩ on (001) surface and ⟨111¯⟩ on (011) surface. The critical shear stress to cause domain switching for PZN-PT crystal is estimated to be approximately 49 MPa for both {110} and {111¯} planes based on theoretical analysis. Generally, the SEAM technique has been successfully demonstrated to be a valid technique for observation of domain structures in single crystal PZN-PTs.

Probing Single Pt Atoms in Complex Intermetallic Al13Fe4.

PubMed

Yamada, Tsunetomo; Kojima, Takayuki; Abe, Eiji; Kameoka, Satoshi; Murakami, Yumi; Gille, Peter; Tsai, An Pang

2018-03-21

The atomic structure of a 0.2 atom % Pt-doped complex metallic alloy, monoclinic Al 13 Fe 4 , was investigated using a single crystal prepared by the Czochralski method. High-angle annular dark-field scanning transmission electron microscopy showed that the Pt atoms were dispersed as single atoms and substituted at Fe sites in Al 13 Fe 4 . Single-crystal X-ray structural analysis revealed that the Pt atoms preferentially substitute at Fe(1). Unlike those that have been reported, Pt single atoms in the surface layers showed lower activity and selectivity than those of Al 2 Pt and bulk Pt for propyne hydrogenation, indicating that the active state of a given single-atom Pt site is strongly dominated by the bonding to surrounding Al atoms.

Growth, crystalline perfection, spectral, thermal and theoretical studies on imidazolium L-tartrate crystals.

PubMed

Meena, K; Muthu, K; Meenatchi, V; Rajasekar, M; Bhagavannarayana, G; Meenakshisundaram, S P

2014-04-24

Transparent optical quality single crystals of imidazolium L-tartrate (IMLT) were grown by conventional slow evaporation solution growth technique. Crystal structure of the as-grown IMLT was determined by single crystal X-ray diffraction analysis. Thermal analysis reveals the purity of the crystal and the sample is stable up to the melting point. Good transmittance in the visible region is observed and the band gap energy is estimated using diffuse reflectance data by the application of Kubelka-Munk algorithm. The powder X-ray diffraction study reveals the crystallinity of the as-grown crystal and it is compared with that of the experimental one. An additional peak in high resolution X-ray diffraction (HRXRD) indicates the presence of an internal structural low angle boundary. Second harmonic generation (SHG) activity of IMLT is significant as estimated by Kurtz and Perry powder technique. HOMO-LUMO energies and first-order molecular hyperpolarizability of IMLT have been evaluated using density functional theory (DFT) employing B3LYP functional and 6-31G(d,p) basis set. The optimized geometry closely resembles the ORTEP. The vibrational patterns present in the molecule are confirmed by FT-IR coinciding with theoretical patterns. Copyright © 2014 Elsevier B.V. All rights reserved.

Exploring contribution of intermolecular interactions in supramolecular layered assembly of naphthyridine co-crystals: Insights from Hirshfeld surface analysis of their crystalline states

NASA Astrophysics Data System (ADS)

Seth, Saikat Kumar; Das, Nirmal Kumar; Aich, Krishnendu; Sen, Debabrata; Fun, Hoong-Kun; Goswami, Shyamaprasad

2013-09-01

Co-crystals of 1a and 1b have been prepared by slow evaporation of the solutions of mixtures of 2,7-dimethyl-1,8-naphthyridine (1), urea (a) and thiourea (b). The structures of the complexes are determined by the single crystal X-ray diffraction and a detailed investigation of the crystal packing and classification of intermolecular interactions is presented by means of Hirshfeld surface analysis which is of considerable current interest in crystal engineering. The X-ray study reveals that the co-crystal formers are envisioned to produce N-H⋯N hydrogen bond as well as N-H⋯O/N-H⋯S pair-wise hydrogen bonds and also the weaker aromatic π⋯π interactions which cooperatively take part in the crystal packing. The recurring feature of the self-assembly in the compounds is the appearance of the molecular ribbon through multiple hydrogen bonding which are further stacked into molecular layers by π⋯π stacking interactions. Hirshfeld surface analysis for visually analyzing intermolecular interactions in crystal structures employing molecular surface contours and 2D Fingerprint plots have been used to examine molecular shapes. Crystal structure analysis supported with the Hirshfeld surface and fingerprint plots enabled the identification of the significant intermolecular interactions.

Crysalis: an integrated server for computational analysis and design of protein crystallization.

PubMed

Wang, Huilin; Feng, Liubin; Zhang, Ziding; Webb, Geoffrey I; Lin, Donghai; Song, Jiangning

2016-02-24

The failure of multi-step experimental procedures to yield diffraction-quality crystals is a major bottleneck in protein structure determination. Accordingly, several bioinformatics methods have been successfully developed and employed to select crystallizable proteins. Unfortunately, the majority of existing in silico methods only allow the prediction of crystallization propensity, seldom enabling computational design of protein mutants that can be targeted for enhancing protein crystallizability. Here, we present Crysalis, an integrated crystallization analysis tool that builds on support-vector regression (SVR) models to facilitate computational protein crystallization prediction, analysis, and design. More specifically, the functionality of this new tool includes: (1) rapid selection of target crystallizable proteins at the proteome level, (2) identification of site non-optimality for protein crystallization and systematic analysis of all potential single-point mutations that might enhance protein crystallization propensity, and (3) annotation of target protein based on predicted structural properties. We applied the design mode of Crysalis to identify site non-optimality for protein crystallization on a proteome-scale, focusing on proteins currently classified as non-crystallizable. Our results revealed that site non-optimality is based on biases related to residues, predicted structures, physicochemical properties, and sequence loci, which provides in-depth understanding of the features influencing protein crystallization. Crysalis is freely available at http://nmrcen.xmu.edu.cn/crysalis/.

Crysalis: an integrated server for computational analysis and design of protein crystallization

PubMed Central

Wang, Huilin; Feng, Liubin; Zhang, Ziding; Webb, Geoffrey I.; Lin, Donghai; Song, Jiangning

2016-01-01

The failure of multi-step experimental procedures to yield diffraction-quality crystals is a major bottleneck in protein structure determination. Accordingly, several bioinformatics methods have been successfully developed and employed to select crystallizable proteins. Unfortunately, the majority of existing in silico methods only allow the prediction of crystallization propensity, seldom enabling computational design of protein mutants that can be targeted for enhancing protein crystallizability. Here, we present Crysalis, an integrated crystallization analysis tool that builds on support-vector regression (SVR) models to facilitate computational protein crystallization prediction, analysis, and design. More specifically, the functionality of this new tool includes: (1) rapid selection of target crystallizable proteins at the proteome level, (2) identification of site non-optimality for protein crystallization and systematic analysis of all potential single-point mutations that might enhance protein crystallization propensity, and (3) annotation of target protein based on predicted structural properties. We applied the design mode of Crysalis to identify site non-optimality for protein crystallization on a proteome-scale, focusing on proteins currently classified as non-crystallizable. Our results revealed that site non-optimality is based on biases related to residues, predicted structures, physicochemical properties, and sequence loci, which provides in-depth understanding of the features influencing protein crystallization. Crysalis is freely available at http://nmrcen.xmu.edu.cn/crysalis/. PMID:26906024

Photoelectrochemical Stability and Alteration Products of n-Type Single-Crystal ZnO Photoanodes

DOE PAGES

Paulauskas, I. E.; Jellison, G. E.; Boatner, L. A.; ...

2011-01-01

The photoelectrochemical stability and surface-alteration characteristics of doped and undoped n-type ZnO single-crystal photoanode electrodes were investigated. The single-crystal ZnO photoanode properties were analyzed using current-voltage measurements plus spectral and time-dependent quantum-yield methods. These measurements revealed a distinct anodic peak and an accompanying cathodic surface degradation process at negative potentials. The features of this peak depended on time and the NaOH concentration in the electrolyte, but were independent of the presence of electrode illumination. Current measurements performed at the peak indicate that charging and discharging effects are apparently taking place at the semiconductor/electrolyte interface. This result is consistent with themore » significant reactive degradation that takes place on the ZnO single crystal photoanode surface and that ultimately leads to the reduction of the ZnO surface to Zn metal. The resulting Zn-metal reaction products create unusual, dendrite-like, surface alteration structural features that were analyzed using x-ray diffraction, energy-dispersive analysis, and scanning electron microscopy. ZnO doping methods were found to be effective in increasing the n-type character of the crystals. Higher doping levels result in smaller depletion widths and lower quantum yields, since the minority carrier diffusion lengths are very short in these materials.« less

Crucibleless crystal growth and Radioluminescence study of calcium tungstate single crystal fiber

NASA Astrophysics Data System (ADS)

Silva, M. S.; Jesus, L. M.; Barbosa, L. B.; Ardila, D. R.; Andreeta, J. P.; Silva, R. S.

2014-11-01

In this article, single phase and high optical quality scheelite calcium tungstate single crystal fibers were grown by using the crucibleless laser heated pedestal growth technique. The as-synthesized calcium tungstate powders used for shaping seed and feed rods were investigated by X-ray diffraction technique. As-grown crystals were studied by Raman spectroscopy and Radioluminescence measurements. The results indicate that in both two cases, calcined powder and single crystal fiber, only the expected scheelite CaWO4 phase was observed. It was verified large homogeneity in the crystal composition, without the presence of secondary phases. The Radioluminescence spectra of the as-grown single crystal fibers are in agreement with that present in Literature for bulk single crystals, presented a single emission band centered at 420 nm when irradiated with β-rays.

Flexible radio-frequency single-crystal germanium switch on plastic substrates

NASA Astrophysics Data System (ADS)

Qin, Guoxuan; Cai, Tianhao; Yuan, Hao-Chih; Seo, Jung-Hun; Ma, Jianguo; Ma, Zhenqiang

2014-04-01

This Letter presents the realization and characterizations of the flexible radio-frequency (RF)/microwave switches on plastic substrates employing single-crystal germanium (Ge) nanomembranes. The fabricated flexible Ge single-pole, single-throw (SPST) switches display high frequency responses (e.g., insertion loss of <1.3 dB at up to 30 GHz and isolation >10 dB at up to ˜13 GHz). RF performance tradeoff exists for the flexible Ge switches and the major affecting parameters are determined. The flexible Ge SPST switch shows better RF property to that of the flexible Si SPST switch. Underlying mechanism is investigated by theoretical analysis and modeling of switches with different structures.

Single crystalline growth of a soluble organic semiconductor in a parallel aligned liquid crystal solvent using rubbing-treated polyimide films

NASA Astrophysics Data System (ADS)

Matsuzaki, Tomoya; Shibata, Yosei; Takeda, Risa; Ishinabe, Takahiro; Fujikake, Hideo

2017-01-01

For directional control of organic single crystals, we propose a crystal growth method using liquid crystal as the solvent. In this study, we examined the formation of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) single crystals using a parallel aligned liquid crystal (LC) cell and rubbing-treated polyimide films in order to clarify the effects of LC alignment on anisotropic C8-BTBT crystal growth. Based on the results, we found that the crystal growth direction of C8-BTBT single crystals was related to the direction of the aligned LC molecules because of rubbing treatment. Moreover, by optical evaluation, we found that the C8-BTBT single crystals have a aligned molecular structure.

Synthesis, crystal structure, Hirshfeld surfaces analysis and anti-ischemic activity of cinnamide derivatives

NASA Astrophysics Data System (ADS)

Zhong, Jian-gang; Han, Jia-pei; Li, Xiao-feng; Xu, Yi; Zhong, Yan; Wu, Bin

2018-02-01

Two cinnamide derivatives, namely, (E)-1-(4-(bis(4-methylphenyl)- methyl)piperazin-1-yl)-3-(3,4-diethoxyphenyl)prop-2-en-1-one (5) and (E)-1-(4-(bis- (4-fluorophenyl)methyl)piperazin-1-yl)-3-(4-methoxyphenyl)prop-2-en-1-one (6), have been synthesized and characterized by IR spectra, High resolution mass spectra, 1H NMR spectra, 13C NMR spectra. The compound 5 is a novel compound and has never been reported in the literature. Their crystal structures were studied by single-crystal X-ray diffraction. They all crystallize in the monoclinic system. The single-crystal X-ray revealed that compound 5 has infinite X-shaped 1-D polymeric chains structure and compound 6 has a layered 3-D structure by intermolecular interactions. Hirshfeld surface analysis demonstrated the presence of H⋯H, O⋯H, C⋯H, F⋯H, Csbnd H⋯π and π⋯π intermolecular interactions. In addition, the MTT assay results indicated that the compounds 5 and 6 display effective activities against neurotoxicity which is induced by glutamine in PC12 cells. The in vivo experiment indicated that the compound 6 has a good protective effect on cerebral infarction.

Integrated nonlinear optical imaging microscope for on-axis crystal detection and centering at a synchrotron beamline

PubMed Central

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.

2013-01-01

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294

Synthesis, characterization, single crystal X-ray and DFT analysis of disubstituted phosphorodithioates

NASA Astrophysics Data System (ADS)

Kour, Mandeep; Kumar, Sandeep; Feddag, Ahmed; Andotra, Savit; Chouaih, Abdelkader; Gupta, Vivek K.; Kant, Rajni; Pandey, Sushil K.

2018-04-01

Disubstituted phosphorodithioates of the type [{(2,5-CH3)2C6H3O}2PS2HNEt3] (1) and [{(3,5-CH3)2C6H3O)2(PS2)}2] (2) were synthesized and characterized by IR and NMR (1H,13C and 31P) spectroscopic studies and as single crystal X-ray analysis. The compound 1 crystallizes in monoclinic space group P21/c whereas compound 2 crystallizes in triclinic space group Pbar1. The X-ray analysis reveals that in compound 1 phosphorus atom is coordinated to the two S and two O atoms to form tetrahedral geometry. The structure is stabilized by cation-anion Nsbnd H⋯S hydrogen bonded interactions. In compound 2, the two phosphorus atoms have a distorted tetrahedral geometry coordinated to two (3,5-CH3)2C6H3O groups. The molecule possesses a crystallographic center of symmetry and consists of zig-zag array of Sdbnd Psbnd Ssbnd Ssbnd Pdbnd S linkages with two diphenyldithiophosphate moieties in the trans configuration. Molecular geometries, HOMO-LUMO analysis and molecular electrostatic potential of compounds 1 and 2 are investigated by theoretical calculations using B3LYP functional with the 6-311G basis combination set in the ground state and compared with the experimental values.

Study of Etching Pits in a Large-grain Single Cell Bulk Niobium Cavity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Xin; Ciovati, Gianluigi; Reece, Charles E.

2009-11-01

Performance of SRF cavities are limited by non-linear localized effects. The variation of local material characters between "hot" and "cold" spots is thus of intense interest. Such locations were identified in a BCP-etched large-grain single-cell cavity and removed for examination by high resolution electron microscopy (SEM), electron-back scattering diffraction microscopy (EBSD), optical microscopy, and 3D profilometry. Pits with clearly discernable crystal facets were observed in both "hotspot" and "coldspot" specimens. The pits were found in-grain, at bi-crystal boundaries, and on tri-crystal junctions. They are interpreted as etch pits induced by surface crystal defects (e.g. dislocations). All "coldspots" examined had qualitativelymore » low density of etching pits or very shallow tri-crystal boundary junction. EBSD revealed crystal structure surrounding the pits via crystal phase orientation mapping, while 3D profilometry gave information on the depth and size of the pits. In addition, a survey of the samples by energy dispersive X-ray analysis (EDX) did not show any significant contamination of the samples surface.« less

Ignition and growth modeling of detonation reaction zone experiments on single crystals of PETN and HMX

NASA Astrophysics Data System (ADS)

White, Bradley W.; Tarver, Craig M.

2017-01-01

It has long been known that detonating single crystals of solid explosives have much larger failure diameters than those of heterogeneous charges of the same explosive pressed or cast to 98 - 99% theoretical maximum density (TMD). In 1957, Holland et al. demonstrated that PETN single crystals have failure diameters of about 8 mm, whereas heterogeneous PETN charges have failure diameters of less than 0.5 mm. Recently, Fedorov et al. quantitatively determined nanosecond time resolved detonation reaction zone profiles of single crystals of PETN and HMX by measuring the interface particle velocity histories of the detonating crystals and LiF windows using a PDV system. The measured reaction zone time durations for PETN and HMX single crystal detonations were approximately 100 and 260 nanoseconds, respectively. These experiments provided the necessary data to develop Ignition and Growth (I&G) reactive flow model parameters for the single crystal detonation reaction zones. Using these parameters, the calculated unconfined failure diameter of a PETN single crystal was 7.5 +/- 0.5 mm, close to the 8 mm experimental value. The calculated failure diameter of an unconfined HMX single crystal was 15 +/- 1 mm. The unconfined failure diameter of an HMX single crystal has not yet been determined precisely, but Fedorov et al. detonated 14 mm diameter crystals confined by detonating a HMX-based plastic bonded explosive (PBX) without initially overdriving the HMX crystals.

Solid-state reaction kinetics of neodymium doped magnesium hydrogen phosphate system

NASA Astrophysics Data System (ADS)

Gupta, Rashmi; Slathia, Goldy; Bamzai, K. K.

2018-05-01

Neodymium doped magnesium hydrogen phosphate (NdMHP) crystals were grown by using gel encapsulation technique. Structural characterization of the grown crystals has been carried out by single crystal X-ray diffraction (XRD) and it revealed that NdMHP crystals crystallize in orthorhombic crystal system with space group Pbca. Kinetics of the decomposition of the grown crystals has been studied by non-isothermal analysis. The estimation of decomposition temperatures and weight loss has been made from the thermogravimetric/differential thermo analytical (TG/DTA) in conjuncture with DSC studies. The various steps involved in the thermal decomposition of the material have been analysed using Horowitz-Metzger, Coats-Redfern and Piloyan-Novikova equations for evaluating various kinetic parameters.

Three-dimensional magnetic critical behavior in CrI 3

DOE PAGES

Liu, Yu; Petrovic, C.

2018-01-18

CrI 3 is a promising candidate for the van der Waals bonded ferromagnetic devices since its ferromagnetism can be maintained upon exfoliating of bulk crystals down to single layer. In this work we studied critical properties of bulk CrI 3 single crystals around the paramagnetic to ferromagnetic phase transition. Critical exponents β= 0.260(4) with a critical temperature T c= 60.05(13) K and γ= 1.136(6) with T c= 60.43(4) K are obtained by the Kouvel-Fisher method, whereas δ= 5.32(2) is obtained by a critical isotherm analysis at T c= 60 K. In conclusion, the critical exponents determined in bulk CrI 3more » single crystals suggest a three-dimensional long-range magnetic coupling with the exchange distance decaying as J(r)≈r -4:69« less

Crystallization and initial X-ray analysis of polyhydroxyalkanoate granule-associated protein from Aeromonas hydrophila

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Minglian; Li, Zhenguo; Zheng, Wei

The phasin PhaP{sub Ah} from A. hydrophila strain 4AK4 was crystallized using the hanging-drop vapour-diffusion method. Polyhydroxyalkanoate (PHA) granule-associated proteins (phasins) were discovered in PHA-accumulating bacteria. They play a crucial role as a structural protein during initial PHA-granule formation and granule growth and also serve as interfaces for granule stabilization in vivo. The phasin PhaP{sub Ah} from Aeromonas hydrophila strain 4AK4 was crystallized using the hanging-drop vapour-diffusion method. Single crystals were cryocooled for X-ray diffraction analysis. The phasin crystals belonged to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 80.8, b = 108.9, c = 134.4 Å.

Growth and characterization of new semiorganic nonlinear optical and piezoelectric lithium sulfate monohydrate oxalate single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, Harsh; Sinha, Nidhi; Kumar, Binay, E-mail: b3kumar69@yahoo.co.in

2015-04-15

Highlights: • A new semiorganic single crystal of LSO grown by slow evaporation technique. • Morphological studies of the LSO crystal deduced by BFDH law. • In the UV–vis spectrum wide transparent region and large band gap were found. • SHG is equal to KDP crystal and d{sub 33} was found to be equal to 6pC/N. • Grown crystal belongs to softer category. - Abstract: New semiorganic crystal of lithium sulfate monohydrate oxalate (LSO) for nonlinear application was synthesized by controlled slow evaporation method. The growth rate of various planes of the grown crystal was estimated by morphological study. Singlemore » crystal XRD analysis confirmed that the crystal belongs to triclinic lattice with space group P1. High transparency (∼95%) with large band gap (4.57 eV) was analyzed by UV–vis studies. FTIR and Raman spectroscopy were used to identify various functional groups present in the LSO crystal. SHG efficiency was found to be equal to the KDP crystal. Thermal stability (up to 117.54 °C) and melting point (242 °C) of the crystal were studied by TG-DTA. In dielectric measurements, the value of dielectric constant decreases with increase in frequency. Hardness studies confirmed soft nature of crystals. The piezoelectric coefficient was found to be 6pC/N along [0 0 1].« less

Ultrathin inorganic molecular nanowire based on polyoxometalates

PubMed Central

Zhang, Zhenxin; Murayama, Toru; Sadakane, Masahiro; Ariga, Hiroko; Yasuda, Nobuhiro; Sakaguchi, Norihito; Asakura, Kiyotaka; Ueda, Wataru

2015-01-01

The development of metal oxide-based molecular wires is important for fundamental research and potential practical applications. However, examples of these materials are rare. Here we report an all-inorganic transition metal oxide molecular wire prepared by disassembly of larger crystals. The wires are comprised of molybdenum(VI) with either tellurium(IV) or selenium(IV): {(NH4)2[XMo6O21]}n (X=tellurium(IV) or selenium(IV)). The ultrathin molecular nanowires with widths of 1.2 nm grow to micrometre-scale crystals and are characterized by single-crystal X-ray analysis, Rietveld analysis, scanning electron microscopy, X-ray photoelectron spectroscopy, ultraviolet–visible spectroscopy, thermal analysis and elemental analysis. The crystals can be disassembled into individual molecular wires through cation exchange and subsequent ultrasound treatment, as visualized by atomic force microscopy and transmission electron microscopy. The ultrathin molecular wire-based material exhibits high activity as an acid catalyst, and the band gap of the molecular wire-based crystal is tunable by heat treatment. PMID:26139011

A 1:1 pharmaceutical cocrystal of myricetin in combination with uncommon piracetam conformer: X-ray single crystal analysis and mechanochemical synthesis

NASA Astrophysics Data System (ADS)

Sowa, Michał; Ślepokura, Katarzyna; Matczak-Jon, Ewa

2014-01-01

Combination of two Active Pharmaceutical Ingredients, myricetin and piracetam, yields a 1:1 cocrystal characterized by X-ray single-crystal and powder diffraction, Raman spectroscopy, 1H NMR, thermal analysis (DSC and TG-DTA) methods. Constituents of the cocrystalline phase were also investigated in terms of Hirshfeld surfaces. Compounds in their neutral forms cocrystallize in the Pna21 space group of orthorhombic system. Notably, piracetam adopts an uncommon conformation, not encountered in its cocrystals previously described. In the crystal lattice, a three-dimensional hydrogen-bonded network is observed, including formation of a 2D molecular scaffolding motif. A scale-up procedure is readily available with use of solvent-drop grinding method, in which application of a variety of common solvents leads to formation of the cocrystal, as confirmed by XRPD and Raman spectroscopy.

Synthesis and crystal structure of an oxovanadium(IV) complex with a pyrazolone ligand and its use as a heterogeneous catalyst for the oxidation of styrene under mild conditions.

PubMed

Parihar, Sanjay; Pathan, Soyeb; Jadeja, R N; Patel, Anjali; Gupta, Vivek K

2012-01-16

1-Phenyl-3-methyl-4-touloyl-5-pyrazolone (ligand) was synthesized and used to prepare an oxovanadium(IV) complex. The complex was characterized by single-crystal X-ray analysis and various spectroscopic techniques. The single-crystal X-ray analysis of the complex shows that the ligands are coordinated in a syn configuration to each other and create a distorted octahedral environment around the metal ion. A heterogeneous catalyst comprising an oxovanadium(IV) complex and hydrous zirconia was synthesized, characterized by various physicochemical techniques, and successfully used for the solvent-free oxidation of styrene. The influence of the reaction parameters (percent loading, molar ratio of the substrate to H(2)O(2), amount of catalyst, and reaction time) was studied. The catalyst was reused three times without any significant loss in the catalytic activity.

Secondary orientation effects in a single crystal superalloy under mechanical and thermal loads

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

1991-01-01

The nickel-base single crystal superalloy PWA 1480 is a candidate blading material for the advanced turbopump development program of the SSME. In order to improve thermal fatigue resistance of the turbine blades, the single crystal superalloy PWA 1480 is grown along the low modulus zone axes (001) crystal orientation by a directional solidification process. Since cubic single crystal materials such as PWA 1480 exhibit anisotropic elastic behavior, the stresses developed within the single crystal superalloy due to mechanical and thermal loads are likely to be affected by the exact orientation of the secondary crystallographic direction with respect to the geometry of the turbine blade. The effects of secondary crystal orientation on the elastic response of single crystal PWA 1480 superalloy were investigated.

Performance of A Compact Multi-crystal High-purity Germanium Detector Array for Measuring Coincident Gamma-ray Emissions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Howard, Chris; Daigle, Stephen; Buckner, Matt

2015-02-18

The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ) 15O* reaction for several transition energies at an effective center of mass energy of 163 keV. Owing to the segmented nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within the uncertainties with the past measurements. Details of the analysis and detector performance will be presented.

Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

PubMed Central

Saghatforoush, L. A.; Valencia, L.; Chalabian, F.; Ghammamy, Sh.

2011-01-01

A new Cd(II) complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy), [Cd(Cltpy)(I)2], has been synthesized and characterized by CHN elemental analysis, 1H-NMR, 13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria. PMID:21738495

A facile approach towards synthesis, characterization, single crystal structure, and DFT study of 5-bromosalicylalcohol

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rastogi, Rupali, E-mail: rastogirupali@ymail.com; Tarannum, Nazia; Butcher, R. J.

2016-03-15

5-Bromosalicylalcohol was prepared by the interaction of NaBH{sub 4} and 5-bromosalicylaldehyde. The use of sodium borohydride makes the reaction easy, facile, economic and does not require any toxic catalyst. The compound is characterized by FTIR, {sup 1}H NMR, {sup 13}C NMR, TEM and ESI-mass spectra. Crystal structure is determined by single crystal X-ray analysis. Quantum mechanical calculations of geometries, energies and thermodynamic parameters are carried out using density functional theory (DFT/B3LYP) method with 6-311G(d,p) basis set. The optimized geometrical parameters obtained by B3LYP method show good agreement with experimental data.

Shock-Induced phase transition of single crystal copper

NASA Astrophysics Data System (ADS)

Neogi, Anupam; Mitra, Nilanjan

2017-05-01

We have carried out a series of multi-million atoms non-equilibrium molecular dynamics simulations to investigate the effect of crystal orientation over the shock induced plasticity and phase transformation in single crystal copper. Crystallographic orientation of [100], [110] and [111] has been studied for various intensity of shock ranging from 1.0 km/s to 3.0 km/s. During shock wave propagation along <100> and <110>, a FCC-to-BCC phase transformation has been observed to occur behind the shock front at higher intensity of shock. Nucleated body centered phase is identified through common neighbor analysis, polyhedral matching template method, radial distribution function and also from the energetic of the particles.

Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite.

PubMed

Yamanaka, Takamitsu

2005-09-01

The bright source and highly collimated beam of synchrotron radiation offers many advantages for single-crystal structure analysis under non-ambient conditions. The structure changes induced by the lattice-electron interaction under high pressure have been investigated using a diamond anvil pressure cell. The pressure dependence of electron density distributions around atoms is elucidated by a single-crystal diffraction study using deformation electron density analysis and the maximum entropy method. In order to understand the bonding electrons under pressure, diffraction intensity measurements of FeTiO3 ilmenite and gamma-SiO2 stishovite single crystals at high pressures were made using synchrotron radiation. Both diffraction studies describe the electron density distribution including bonding electrons and provide the effective charge of the cations. In both cases the valence electrons are more localized around the cations with increasing pressure. This is consistent with molecular orbital calculations, proving that the bonding electron density becomes smaller with pressure. The thermal displacement parameters of both samples are reduced with increasing pressure.

Piezoelectric single crystals for ultrasonic transducers in biomedical applications

PubMed Central

Zhou, Qifa; Lam, Kwok Ho; Zheng, Hairong; Qiu, Weibao; Shung, K. Kirk

2014-01-01

Piezoelectric single crystals, which have excellent piezoelectric properties, have extensively been employed for various sensors and actuators applications. In this paper, the state–of–art in piezoelectric single crystals for ultrasonic transducer applications is reviewed. Firstly, the basic principles and design considerations of piezoelectric ultrasonic transducers will be addressed. Then, the popular piezoelectric single crystals used for ultrasonic transducer applications, including LiNbO3 (LN), PMN–PT and PIN–PMN–PT, will be introduced. After describing the preparation and performance of the single crystals, the recent development of both the single–element and array transducers fabricated using the single crystals will be presented. Finally, various biomedical applications including eye imaging, intravascular imaging, blood flow measurement, photoacoustic imaging, and microbeam applications of the single crystal transducers will be discussed. PMID:25386032

Structural and photoluminescence studies on europium-doped lithium tetraborate (Eu:Li2B4O7) single crystal grown by microtube Czochralski (μT-Cz) technique

NASA Astrophysics Data System (ADS)

A, Kumaresh; R, Arun Kumar; N, Ravikumar; U, Madhusoodanan; B, S. Panigrahi; K, Marimuthu; M, Anuradha

2016-05-01

Rare earth europium (Eu3+)-doped lithium tetraborate (Eu:Li2B4O7) crystal is grown from its stoichiometric melt by microtube Czochralski pulling technique (μT-Cz) for the first time. The grown crystals are subjected to powder x-ray diffraction (PXRD) analysis which reveals the tetragonal crystal structure of the crystals. UV-vis-NIR spectral analysis is carried out to study the optical characteristics of the grown crystals. The crystal is transparent in the entire visible region, and the lower cutoff is observed to be at 304 nm. The existence of BO3 and BO4 bonding structure and the molecular associations are analyzed by Fourier transform infrared (FTIR) spectroscopy. The results of excitation and emission-photoluminescence spectra of europium ion incorporated in lithium tetraborate (LTB) single crystal reveal that the observations of peaks at 258, 297, and 318 nm in the excitation spectra and peaks at 579, 591, 597, 613, and 651 nm are observed in the emission spectra. The chromaticity coordinates are calculated from the emission spectra, and the emission intensity of the grown crystal is characterized through a CIE 1931 (Commission International d’Eclairage) color chromaticity diagram. Project supported by the Department of Science and Technology-Science and Engineering Research Board (Grant No. SR/S2/LOP-0012/2011), the Government of India for Awarding Major Research Project, the University Grants Commission-Department of Atomic Research-Consortium for Scientific Research (Grant No. CSR-KN/CSR-63/2014-2015/503), and the Kalpakkam and Indore, India.

Growth, structural, spectral, mechanical, thermal and dielectric characterization of phosphoric acid admixtured L-alanine (PLA) single crystals.

PubMed

Rose, A S J Lucia; Selvarajan, P; Perumal, S

2011-10-15

Phosphoric acid admixtured L-alanine (PLA) single crystals were grown successfully by solution method with slow evaporation technique at room temperature. Crystals of size 18 mm×12 mm×8 mm have been obtained in 28 days. The grown crystals were colorless and transparent. The solubility of the grown samples has been found out at various temperatures. The lattice parameters of the grown crystals were determined by X-ray diffraction technique. The reflection planes of the sample were confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. Fourier transform infrared (FTIR) studies were used to confirm the presence of various functional groups in the crystals. UV-visible transmittance spectrum was recorded to study the optical transparency of grown crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz-Perry powder technique and a study of its second harmonic generation efficiency in comparison with potassium dihydrogen phosphate (KDP) has been made. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to thermo gravimetric and differential thermal analysis (TG/DTA). The dielectric behavior of the sample was also studied. Copyright © 2011 Elsevier B.V. All rights reserved.

Preparation of a Non-Polar ZnO Film on a Single-Crystal NdGaO3 Substrate by the RF Sputtering Method

NASA Astrophysics Data System (ADS)

Kashiwaba, Y.; Tanaka, Y.; Sakuma, M.; Abe, T.; Imai, Y.; Kawasaki, K.; Nakagawa, A.; Niikura, I.; Kashiwaba, Y.; Osada, H.

2018-04-01

Preparation of non-polar ZnO ( 11\\overline{2} 0 ) films on single-crystal NdGaO3 (NGO) (001) substrates was successfully achieved by the radio frequency (RF) sputtering method. Orientation, deposition rate, and surface roughness of ZnO films strongly depend on the working pressure. Characteristics of ZnO films deposited on single-crystal NGO (001) substrates were compared with those of ZnO films deposited on single-crystal sapphire ( 01\\overline{1} 2 ) substrates. An x-ray diffraction peak of the ZnO ( 11\\overline{2} 0 ) plane was observed on ZnO films deposited on single-crystal NGO (001) substrates under working pressure of less than 0.5 Pa. On the other hand, uniaxially oriented ZnO ( 11\\overline{2} 0 ) films on single-crystal sapphire ( 01\\overline{1} 2 ) substrates were observed under working pressure of 0.1 Pa. The mechanism by which the diffraction angle of the ZnO ( 11\\overline{2} 0 ) plane on single-crystal NGO (001) substrates was shifted is discussed on the basis of anisotropic stress of lattice mismatch. The deposition rate of ZnO films decreased with an increase in working pressure, and the deposition rate on single-crystal NGO (001) substrates was larger than that on single-crystal sapphire ( 01\\overline{1} 2 ) substrates. Root mean square (RMS) roughness of ZnO films increased with an increase in working pressure, and RMS roughness of ZnO films on single-crystal NGO (001) substrates was smaller than that of ZnO films on single-crystal sapphire ( 01\\overline{1} 2 ) substrates even though the film thickness on single-crystal NGO (001) substrates was greater than that on sapphire substrates. It is thought that a single-crystal NGO (001) substrate is useful for deposition of non-polar ZnO ( 11\\overline{2} 0 ) films.

Single crystal growth, characterization and high-pressure Raman spectroscopy of impurity-free magnesite (MgCO3)

NASA Astrophysics Data System (ADS)

Liang, Wen; Li, Zeming; Yin, Yuan; Li, Rui; Chen, Lin; He, Yu; Dong, Haini; Dai, Lidong; Li, Heping

2018-05-01

The understanding of the physical and chemical properties of magnesite (MgCO3) under deep-mantle conditions is highly important to capture the essence of deep-carbon storage in Earth's interior. To develop standard rating scales, the impurity-free magnesite single crystal, paying particular attention to the case of avoiding adverse impacts of Ca2+, Fe2+, and Mn2+ impurities in natural magnesite, is undoubtedly necessary for all research of magnesite, including crystalline structural phase transitions, anisotropic elasticity and conductivity, and equation of state (EoS). Thus, a high-quality single crystal of impurity-free magnesite was grown successfully for the first time using the self-flux method under high pressure-temperature conditions. The size of the magnesite single crystal, observed in a plane-polarized microscope, exceeds 200 μm, and the crystal exhibits a rhombohedral structure to cleave along the (101) plane. In addition, its composition of Mg0.999 ± 0.001CO3 was quantified through electron probing analysis. The structural property was investigated by means of single crystal X-ray diffraction and the unit cell dimensions obtained in the rhombohedral symmetry of the R\\bar {3}c space group are a = 4.6255 (3) and c = 14.987 (2), and the final R = 0.0243 for 718 reflections. High-pressure Raman spectroscopy of the magnesite single crystal was performed up to 27 GPa at ambient temperature. All Raman active bands, ν i, without any splitting increased almost linearly with increasing pressure. In combination with the high-pressure Raman results {{d/ν _i}}{{{d}P}} and the bulk modulus K T (103 GPa) reported from magnesite EoS studies, the mode Grüneisen parameters (1.49, 1.40, 0.26, and 0.27) of each vibration ( T, L, ν 4, and ν 1) were calculated.

Electrical characteristics of organic perylene single-crystal-based field-effect transistors

NASA Astrophysics Data System (ADS)

Lee, Jin-Woo; Kang, Han-Saem; Kim, Min-Ki; Kim, Kihyun; Cho, Mi-Yeon; Kwon, Young-Wan; Joo, Jinsoo; Kim, Jae-Il; Hong, Chang-Seop

2007-12-01

We report on the fabrication of organic field-effect transistors (OFETs) using perylene single crystal as the active material and their electrical characteristics. Perylene single crystals were directly grown from perylene powder in a furnace using a relatively short growth time of 1-3 h. The crystalline structure of the perylene single crystals was characterized by means of a single-crystal x-ray diffractometer. In order to place the perylene single crystal onto the Au electrodes of the field-effect transistor, a polymethlymethacrylate thin layer was spin-coated on top of the crystal surface. The OFETs fabricated using the perylene single crystal showed a typical p-type operating mode. The field-effect mobility of the perylene crystal based OFETs was measured to be ˜9.62×10-4 cm2/V s at room temperature. The anisotropy of the mobility implying the existence of different mobilities when applying currents in different directions was observed for the OFETs, and the existence of traps in the perylene crystal was found through the measurements of the temperature-dependent mobility at various operating drain voltages.

Crystallization and preliminary X-ray diffraction analysis of central structure domains from mumps virus F protein

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yueyong; Xu, Yanhui; Zhu, Jieqing

2005-09-01

Single crystals of the central structure domains from mumps virus F protein have been obtained by the hanging-drop vapour-diffusion method. A diffraction data set has been collected to 2.2 Å resolution. Fusion of members of the Paramyxoviridae family involves two glycoproteins: the attachment protein and the fusion protein. Changes in the fusion-protein conformation were caused by binding of the attachment protein to the cellular receptor. In the membrane-fusion process, two highly conserved heptad-repeat (HR) regions, HR1 and HR2, are believed to form a stable six-helix coiled-coil bundle. However, no crystal structure has yet been determined for this state in themore » mumps virus (MuV, a member of the Paramyxoviridae family). In this study, a single-chain protein consisting of two HR regions connected by a flexible amino-acid linker (named 2-Helix) was expressed, purified and crystallized by the hanging-drop vapour-diffusion method. A complete X-ray data set was obtained in-house to 2.2 Å resolution from a single crystal. The crystal belongs to space group C2, with unit-cell parameters a = 161.2, b = 60.8, c = 40.1 Å, β = 98.4°. The crystal structure will help in understanding the molecular mechanism of Paramyxoviridae family membrane fusion.« less

Luminescence and Excitation Spectra of U 3+ doped RbY 2 Cl 7 Single Crystals

DOE PAGES

Karbowiak, M.; Murdoch, K.; Drożdżyński, J.; ...

1996-08-01

Uranium(3+) doped single crystals of RbY 2 Cl 7 with a uranium concentration of 0.05% and 0.2% were grown by the Bridgman-Stockbarger method using RbU 2 Cl 7 as the doping substance. Polished plates of ca. 5 mm in diameter were used for measurements of luminescence and excitation spectra. And since the U 3+ ions occupy two somewhat different site symmetries, a splitting of all observed f-f bands was observed. Furthermore, the analysis of the spectra enabled definitively an assignment of 22 crystal field bands for both site symmetries as well as the total crystal field splitting of the groundmore » level, equal to 473 cm -1 and 567 cm -1 for the first and second site symmetry, respectively.« less

Synthesis and characterization of a prominent NLO active MOF of lead with 1,5-naphthalenedisulfonic acid

NASA Astrophysics Data System (ADS)

Prasad, S. Shibu; Sudarsanakumar, M. R.; Dhanya, V. S.; Suma, S.; Kurup, M. R. Prathapachandra

2018-09-01

A new metal-organic framework of lead, [Pb(1,5-nds)(H2O)3]n (1,5-nds = 1,5-naphthalenedisulfonate) having prominent nonlinear optical property has been prepared by single gel diffusion technique at ambient condition using sodium metasilicate. The second harmonic generation efficiency was analyzed using Kurtz and Perry powder method and was found to be 30 times as large as potassium dihydrogen phosphate (KDP). Single crystal X-ray diffraction studies reveal the crystal structure. The grown crystals were further characterized by elemental analysis, powder XRD study, thermogravimetry, FT-IR and UV-visible spectral studies. The Pb2S2O4 rings in the crystal structure form a 1D channel. Hydrogen bonding and π-π interactions provide additional stability to the compound. Photoluminescence studies were also carried out.

Effect of Slag Composition on the Crystallization Kinetics of Synthetic CaO-SiO2-Al2O3-MgO Slags

NASA Astrophysics Data System (ADS)

Esfahani, Shaghayegh; Barati, Mansoor

2018-04-01

The crystallization kinetics of CaO-SiO2-Al2O3-MgO (CSAM) slags was studied with the aid of single hot thermocouple technique (SHTT). Kinetic parameters such as the Avrami exponent ( n), rate coefficient ( K), and effective activation energy of crystallization ( E A ) were obtained by kinetic analysis of data obtained from in situ observation of glassy to crystalline transformation and image analysis. Also, the dependence of nucleation and growth rates of crystalline phases were quantified as a function of time, temperature, and slag basicity. Together with the observations of crystallization front, they facilitated establishing the dominant mechanisms of crystallization. In an attempt to predict crystallization rate under non-isothermal conditions, a mathematical model was developed that employs the rate data of isothermal transformation. The model was validated by reproducing an experimental continuous cooling transformation diagram purely from isothermal data.

Synthesis and structure identification of 2-amino-4, 6- dimethyl pyrimidine with gallic acid and pimelic acid

NASA Astrophysics Data System (ADS)

Mekala, R.; Jagdish, P.; Mathammal, R.

2018-07-01

Reaction of 2-amino-4, 6- dimethyl pyrimidine with carboxylic acid such as gallic acid and pimelic acid, yielded a salt and co-crystal, respectively. The new crystal forms were obtained from slow evaporation technique. The crystal structure and hydrogen bond interaction of the two crystals were determined by single X-ray diffraction analysis. Inter molecular interactions of the compounds were investigated using the 3D Hirshfeld surfaces and the associated 2D fingerprint plots. The functional groups were identified by the FTIR, FT-Raman spectral studies. The presence of carbon and hydrogen in the two samples were identified by the 1H and 13C NMR analysis. The excited energy was observed using UV-Visible spectral analysis. The fluorescence spectra revealed the emission state of the two samples. The thermal behaviour and stability of the two compounds were evaluated by the TGA-DSC analysis.

Probing the magnetic ground state of single crystalline Ce3TiSb5

NASA Astrophysics Data System (ADS)

Matin, M.; Kulkarni, R.; Thamizhavel, A.; Dhar, S. K.; Provino, A.; Manfrinetti, P.

2017-04-01

Motivated by the report of superconductivity in R3TiSb5 (R  =  La and Ce) and possibly Nd3TiSb5 at  ∼4 K, we grew single crystals of La3TiSb5 and Ce3TiSb5 by the high-temperature solution method using Sn as a flux. While in both compounds we observed a superconducting transition at 3.7 K for resistivity and low-field magnetization, our data conclusively show that it arose from residual Sn flux present in the single crystals. In particular, the heat capacity data do not present any of the anomalies expected from a bulk superconducting transition. The anisotropic magnetic properties of Ce3TiSb5, crystallizing in a hexagonal P63/mcm structure, were studied in detail. We find that the Ce ions in Ce3TiSb5 form a Kondo lattice and exhibited antiferromagnetic ordering at 5.5 K with a reduced moment and a moderately normalized Sommerfeld coefficient of 598 mJ/mol K2. The characteristic single-ion Kondo energy scale was found to be  ∼8 K. The magnetization data were subjected to a crystal electric field (CEF) analysis. The experimentally observed Schottky peak in the 4f-electron heat capacity of Ce3TiSb5 was reproduced fairly well by the energy levels derived from the CEF analysis.

Crystal growth and piezoelectric properties of Ca3Ta(Ga0.9Sc0.1)3Si2O14 bulk single crystal

NASA Astrophysics Data System (ADS)

Igarashi, Yu; Yokota, Yuui; Ohashi, Yuji; Inoue, Kenji; Yamaji, Akihiro; Shoji, Yasuhiro; Kamada, Kei; Kurosawa, Shunsuke; Yoshikawa, Akira

2018-03-01

Ca3Ta(Ga0.9Sc0.1)3Si2O14 langasite-type single crystal with a diameter of 1 in. was grown by Czochralski (Cz) method. Obtained crystal had good crystallinity and its lattice constants exceeded those of Ca3TaGa3Si2O14 (CTGS) according to the X-ray analysis. A crack-free specimen cut from the grown crystal was used for the measurements of dielectric constant ε11T/ε0, electromechanical coupling factor k12, and piezoelectric constant d11. The accuracies of these measurements were better than those for the crystal grown by micro-pulling-down (μ-PD) method. Substitution of Ga with Sc resulted modification of these constants in the directions opposite to those observed after partial substitution of Ga (of CTGS) with Al. This suggests that increase of |d14| was most probably associated with enlargement of average size of the Ga sites. The crystal reported here had greater dimensions as compared to analogous crystals grown by the μ-PD method. As a result, accuracy of determination of acoustic constants of this material may be improved.

Exploring the folding pattern of a polymer chain in a single crystal by combining single-molecule force spectroscopy and steered molecular dynamics simulations.

PubMed

Song, Yu; Feng, Wei; Liu, Kai; Yang, Peng; Zhang, Wenke; Zhang, Xi

2013-03-26

Understanding the folding pattern of a single polymer chain within its single crystal will shed light on the mechanism of crystallization. Here, we use the combined techniques of atomic force microscopy (AFM)-based single-molecule force spectroscopy (SMFS) and steered molecular dynamics (SMD) simulations to study the folding pattern of a polyethylene oxide (PEO) chain in its single crystal. Our results show that the folding pattern of a PEO chain in the crystal formed in dilute solution follows the adjacent re-entry folding model. While in the crystal obtained from the melt, the nonadjacent folding with large and irregular loops contributes to big force fluctuations in the force-extension curves. The method established here can offer a novel strategy to directly unravel the chain-folding pattern of polymer single crystals at single-molecule level.

Effect of amaranth dye on the growth and properties of conventional and SR method grown KAP single crystals

NASA Astrophysics Data System (ADS)

Babu Rao, G.; P., Rajesh; Ramasamy, P.

2018-04-01

The 0.1 mol% amaranth added KAP single crystals were grown from aqueous solutions by both slow evaporation solution technique and Sankaranarayanan-Ramasamy method. The single crystal having dimension of 45 mm length and 12 mm diameter was grown with growth rate of 1.5 mm/day using SR method. 87 % transmittance is obtained for SR method grown amaranth added KAP single crystal. The high intense luminescence at 661 nm is obtained from amaranth added conventional and SR method grown KAP single crystal. The amaranth added KAP single crystal possesses good mechanical and laser damage threshold stability.

π-π-Induced aggregation and single-crystal fluorescence anisotropy of 5,6,10b-tri-aza-acephenanthrylene.

PubMed

Ostrowska, Katarzyna; Ceresoli, Davide; Stadnicka, Katarzyna; Gryl, Marlena; Cazzaniga, Marco; Soave, Raffaella; Musielak, Bogdan; Witek, Łukasz J; Goszczycki, Piotr; Grolik, Jarosław; Turek, Andrzej M

2018-05-01

The structural origin of absorption and fluorescence anisotropy of the single crystal of the π-conjugated heterocyclic system 5,6,10b-tri-aza-acephenan-thrylene, TAAP, is presented in this study. X-ray analysis shows that the crystal framework in the space group P [Formula: see text] is formed by centrosymmetric dimers of face-to-face mutually oriented TAAP molecules joined by π-π non-covalent interactions. The conformation of the TAAP molecule is stabilized by intramolecular C-H⋯N( sp 2 ), N( sp 2 )H⋯π(CN), and C-H⋯O( sp 2 ) hydrogen bonds. The presence of weak π-π interactions is confirmed by quantum theory of atoms in molecules (QTAIM) and non-covalent interaction (NCI) analysis. The analysis of the optical spectra of TAAP in solution and in the solid state does not allow the specification of the aggregation type. DFT calculations for the dimer in the gas phase indicate that the lowest singlet excitation is forbidden by symmetry, suggesting H-type aggregation, even though the overall absorption spectrum is bathochromically shifted as for the J-type. The experimental determination of the permanent dipole moment of a TAAP molecule in 1,4-dioxane solution indicates the presence of the monomer form. The calculated absorption and emission spectra of the crystal in a simple approximation are consistent with the experimentally determined orientation of the absorption and emission transition dipole moments in TAAP single crystals. The electrostatic interaction between monomers with a permanent dipole moment ( ca 4 D each) could result in the unusual spectroscopic JH-aggregate behaviour of the TAAP dimer.

Identification of Zn-vacancy-hydrogen complexes in ZnO single crystals: A challenge to positron annihilation spectroscopy

NASA Astrophysics Data System (ADS)

Brauer, G.; Anwand, W.; Grambole, D.; Grenzer, J.; Skorupa, W.; Čížek, J.; Kuriplach, J.; Procházka, I.; Ling, C. C.; So, C. K.; Schulz, D.; Klimm, D.

2009-03-01

A systematic study of various, nominally undoped ZnO single crystals, either hydrothermally grown (HTG) or melt grown (MG), has been performed. The crystal quality has been assessed by x-ray diffraction, and a comprehensive estimation of the detailed impurity and hydrogen contents by inductively coupled plasma mass spectrometry and nuclear reaction analysis, respectively, has been made also. High precision positron lifetime experiments show that a single positron lifetime is observed in all crystals investigated, which clusters at 180-182 ps and 165-167 ps for HTG and MG crystals, respectively. Furthermore, hydrogen is detected in all crystals in a bound state with a high concentration (at least 0.3at.% ), whereas the concentrations of other impurities are very small. From ab initio calculations it is suggested that the existence of Zn-vacancy-hydrogen complexes is the most natural explanation for the given experimental facts at present. Furthermore, the distribution of H at a metal/ZnO interface of a MG crystal, and the H content of a HTG crystal upon annealing and time afterward has been monitored, as this is most probably related to the properties of electrical contacts made at ZnO and the instability in p -type conductivity observed at ZnO nanorods in literature. All experimental findings and presented theoretical considerations support the conclusion that various types of Zn-vacancy-hydrogen complexes exist in ZnO and need to be taken into account in future studies, especially for HTG materials.

Accurate determination of chemical shift tensor orientations of single-crystals by solid-state magic angle spinning NMR

NASA Astrophysics Data System (ADS)

Avadhut, Yamini S.; Weber, Johannes; Schmedt auf der Günne, Jörn

2017-09-01

An improved implementation of single-crystal magic-angle-spinning (MAS) NMR is presented which gives access to chemical shift tensors both in orientation (relative to the crystal axis system) and principal axis values. For mounting arbitrary crystals inside ordinary MAS rotors, a mounting tool is described which allows to relate the crystal orientation determined by diffraction techniques to the rotor coordinate system. The crystal is finally mounted into a MAS rotor equipped with a special insert which allows a defined reorientation of the single-crystal by 90°. The approach is based on the idea that the dispersive spectra, which are obtained when applying read-pulses at specific rotor-phases, not only yield the size of the eigenvalues but also encode the orientation of the different chemical shift (rank-2) tensors. For this purpose two 2D-data sets with orthogonal crystal orientation are fitted simultaneously. The presented analysis for chemical shift tensors is supported by an analytical formula which allows fast calculation of phase and amplitude of individual spinning side-bands and by a protocol which solves the problem of finding the correct reference phase of the spectrum. Different rotor-synchronized pulse-sequences are introduced for the same reason. Experiments are performed on L-alanine and O-phosphorylethanolamine and the observed errors are analyzed in detail. The experimental data are opposed to DFT-computed chemical shift tensors which have been obtained by the extended embedded ion method.

Quasi van der Waals epitaxy of copper thin film on single-crystal graphene monolayer buffer

NASA Astrophysics Data System (ADS)

Lu, Zonghuan; Sun, Xin; Washington, Morris A.; Lu, Toh-Ming

2018-03-01

Quasi van der Waals epitaxial growth of face-centered cubic Cu (~100 nm) thin films on single-crystal monolayer graphene is demonstrated using thermal evaporation at an elevated substrate temperature of 250 °C. The single-crystal graphene was transferred to amorphous (glass) and crystalline (quartz) SiO2 substrates for epitaxy study. Raman analysis showed that the thermal evaporation method had minimal damage to the graphene lattice during the Cu deposition. X-ray diffraction and electron backscatter diffraction analyses revealed that both Cu films are single-crystal with (1 1 1) out-of-plane orientation and in-plane Σ3 twin domains of 60° rotation. The crystallinity of the SiO2 substrates has a negligible effect on the Cu crystal orientation during the epitaxial growth, implying the strong screening effect of graphene. We also demonstrate the epitaxial growth of polycrystalline Cu on a commercial polycrystalline monolayer graphene consisting of two orientation domains offset 30° to each other. It confirms that the crystal orientation of the epitaxial Cu film follows that of graphene, i.e. the Cu film consists of two orientation domains offset 30° to each other when deposited on polycrystalline graphene. Finally, on the contrary to the report in the literature, we show that the direct current and radio frequency flip sputtering method causes significant damage to the graphene lattice during the Cu deposition process, and therefore neither is a suitable method for Cu epitaxial growth on graphene.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.

Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ~10 3–10 4-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering andmore » analysis of phenylalanine hydroxylase fromChromobacterium violaceumcPAH,Trichinella spiralisdeubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied.« less

Syntheses, structural characterization, and DPPH radical scavenging activity of cocrystals of caffeine with 1- and 2-naphthoxyacetic acids

NASA Astrophysics Data System (ADS)

Suresh Kumar, G. S.; Seethalakshmi, P. G.; Sumathi, D.; Bhuvanesh, N.; Kumaresan, S.

2013-03-01

Caffeine:1-naphthoxyacetic acid [(caf)(1-naa)] and caffeine:2-naphthoxyacetic acid [(caf)(2-naa)] cocrystals have been synthesized and single crystals were grown by slow evaporation technique. The structures of the grown crystals were elucidated using single crystal X-ray diffraction analysis. Both the cocrystals belong to the monoclinic crystallographic system with space group P21/c, Z = 4, and α = γ = 90°, whereas β = 111.4244(18)° for [(caf)(1-naa)] and β = 109.281(6)° for [(caf)(2-naa)]. The crystal packing is predominantly stabilized by hydrogen bonding and π-π stacking interactions. The presence of unionized -COOH functional group in both the cocrystals was identified by FTIR spectral analysis. Thermal behavior and stability of both the cocrystals were studied by TGA/DTA analyses. Solvent-free formation of these cocrystals was confirmed by powder X-ray diffraction analyses. The theoretical energy of cocrystals showed that the formers have higher energy than cocrystals 1 and 2. DPPH radical scavenging activity of cocrystals 1 and 2 is slightly greater than the formers.

Spectroscopic investigations using density functional theory on 2-methoxy- 4(phenyliminomethyl)phenol: A non linear optical material

NASA Astrophysics Data System (ADS)

Hijas, K. M.; Madan Kumar, S.; Byrappa, K.; Geethakrishnan, T.; Jeyaram, S.; Nagalakshmi, R.

2018-03-01

Single crystals of 2-methoxy-4(phenyliminomethyl)phenol were grown from ethanol by slow evaporation solution growth technique. Single crystal X-ray diffraction experiment reveals the crystallization in orthorhombic system having non-centrosymmetric space group C2221. Geometrical optimization by density functional theory method was carried out using Gaussian program and compared with experimental results. Detailed experimental and theoretical vibrational analyses were carried out and the results were correlated to find close agreement. Thermal analyses show the material is thermally stable with a melting point of 159 °C. Natural bond orbital analysis was carried out to explain charge transfer interactions through hydrogen bonding. Relatively smaller HOMO-LUMO band gap favors the non linear optical activity of the molecule. Natural population analysis and molecular electrostatic potential calculations visualize the charge distribution in an isolated molecule. Calculated first-order molecular hyperpolarizability and preliminary second harmonic generation test carried out using Kurtz-Perry technique establish 2-methoxy-4(phenyliminomethyl)phenol crystal as a good non linear optical material. Z-scan proposes the material for reverse saturable absorption.

Synthesis aspects, structural, spectroscopic, antimicrobial and room temperature ferromagnetism of zinc iodide complex with Schiff based ligand.

PubMed

Shakila, K; Kalainathan, S

2015-01-25

In this paper, we report the successful growth of complex compound of zinc iodide with thiocarbamide by slow evaporation method. The single crystal XRD study reveals that the crystal belongs to monoclinic system with centrosymmetric space group and powder XRD analysis shows that the perfect crystalline nature of the crystal. The presence of functional group and element were confirmed from FT-IR and EDAX analysis. Optical absorbance of the grown crystal was studied by UV-Vis spectrophotometer. The optical constants were calculated from the optical absorbance data such as refractive index (n), extinction coefficient (K) and reflectance (R). The optical band gap (Eg) of thiocarbamide zinc iodide crystal is 4.22 eV. The magnetic properties of grown crystal have been determined by Vibrating Sample Magnetometry (VSM). Room temperature magnetization revealed a ferromagnetic behaviour for the grown crystal. The antibacterial and antifungal activities of the title compound were performed by well diffusion method and MIC method against the standard bacteria like Staphylococcus aureus, Escherichia coli, Klebsiella pneumonia and against fungus like Aspergillus niger, Rhizopus sps and Penicillium sps. Thermal behaviour of the crystal has been investigated using thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Copyright © 2014. Published by Elsevier B.V.

Nanoimprinted photonic crystal color filters for solar-powered reflective displays.

PubMed

Cho, Eun-Hyoung; Kim, Hae-Sung; Sohn, Jin-Seung; Moon, Chang-Youl; Park, No-Cheol; Park, Young-Pil

2010-12-20

A novel concept for reflective displays that uses two-dimensional photonic crystals with subwavelength gratings is introduced. A solar-powered reflective display with photonic crystal color filters was analyzed by a theoretical approach. We fabricated the photonic crystal color filters on a glass substrate by using low-cost nanoimprint lithography and multi-scan excimer laser annealing to produce RGB color filters through a single patterning process. The theoretical and experimental results show that the color filters have high reflectance and angular tolerance, which was qualitatively confirmed by chromaticity coordination analysis.

High-pressure crystal growth and electromagnetic properties of 5d double-perovskite Ca3OsO6

NASA Astrophysics Data System (ADS)

Feng, Hai Luke; Shi, Youguo; Guo, Yanfeng; Li, Jun; Sato, Akira; Sun, Ying; Wang, Xia; Yu, Shan; Sathish, Clastin I.; Yamaura, Kazunari

2013-05-01

Single crystals of the osmium-containing compound Ca3OsO6 have been successfully grown under high-pressure conditions, for the first time. The crystal structure of Ca3OsO6 were characterized as an ordered double-perovskite structure of space group P21/n with the Ca and Os atoms being fully ordered at the perovskite B-site. The electromagnetic analysis shows that the crystal exhibits a semiconductor-like behavior below 300 K and undergoes an antiferromagnetic transition at 50 K.

Synthesis and crystal structure analysis of uranyl triple acetates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klepov, Vladislav V., E-mail: vladislavklepov@gmail.com; Department of Chemistry, Samara National Research University, 443086 Samara; Serezhkina, Larisa B.

2016-12-15

Single crystals of triple acetates NaR[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O (R=Mg, Co, Ni, Zn), well-known for their use as reagents for sodium determination, were grown from aqueous solutions and their structural and spectroscopic properties were studied. Crystal structures of the mentioned phases are based upon (Na[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}){sup 2–} clusters and [R(H{sub 2}O){sub 6}]{sup 2+} aqua-complexes. The cooling of a single crystal of NaMg[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O from 300 to 100 K leads to a phase transition from trigonal to monoclinic crystal system. Intermolecular interactions between the structural units and their mutual packing were studiedmore » and compared from the point of view of the stereoatomic model of crystal structures based on Voronoi-Dirichlet tessellation. Using this method we compared the crystal structures of the triple acetates with Na[UO{sub 2}(CH{sub 3}COO){sub 3}] and [R(H{sub 2}O){sub 6}][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} and proposed reasons of triple acetates stability. Infrared and Raman spectra were collected and their bands were assigned. - Graphical abstract: Single crystals of uranium based triple acetates, analytical reagents for sodium determination, were synthesized and structurally, spectroscopically and topologically characterized. The structures were compared with the structures of compounds from preceding families [M(H{sub 2}O){sub 6})][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} (M = Mg, Co, Ni, Zn) and Na[UO{sub 2}(CH{sub 3}COO){sub 3}]. Analysis was performed with the method of molecular Voronoi-Dirichlet polyhedra to reveal a large contribution of the hydrogen bonds into intermolecular interactions which can be a reason of low solubility of studied complexes.« less

Q-space analysis of light scattering by ice crystals

NASA Astrophysics Data System (ADS)

Heinson, Yuli W.; Maughan, Justin B.; Ding, Jiachen; Chakrabarti, Amitabha; Yang, Ping; Sorensen, Christopher M.

2016-12-01

Q-space analysis is applied to extensive simulations of the single-scattering properties of ice crystals with various habits/shapes over a range of sizes. The analysis uncovers features common to all the shapes: a forward scattering regime with intensity quantitatively related to the Rayleigh scattering by the particle and the internal coupling parameter, followed by a Guinier regime dependent upon the particle size, a complex power law regime with incipient two dimensional diffraction effects, and, in some cases, an enhanced backscattering regime. The effects of significant absorption on the scattering profile are also studied. The overall features found for the ice crystals are similar to features in scattering from same sized spheres.

Temperature and electric-field induced phase transition behavior and electrical properties of [001]-oriented 0.23Pb(In1/2Nb1/2)O3-0.47Pb(Mg1/3Nb2/3)O3-0.3PbTiO3-Mn single crystals

NASA Astrophysics Data System (ADS)

Zhang, Zhang; Chen, Jianwei; Xu, Jialin; Li, Xiaobing; Luo, Haosu

2017-12-01

The temperature and electric-field induced phase transition behavior and dielectric, piezoelectric, and ferroelectric properties of [001]-oriented 0.23Pb(In1/2Nb1/2)O3-0.47Pb(Mg1/3Nb2/3)O3-0.3PbTiO3-Mn (PIMNT-Mn) single crystals were investigated. Dielectric performance analysis and temperature-dependent Raman spectra show three apparent ferroelectric phase transition temperatures around 120 °C(TR-M),145 °C(TM-T), and 170 °C(TT-C), respectively. In addition, the temperature dependence of the relative Raman intensities of Lorentzian peaks indicates the poled PIMNT-Mn single crystals exhibit rhombohedral(R) → monoclinic(M) → tetragonal(T) → cubic(C) phase transition path. The electrical properties of the PIMNT-Mn single crystals such as the longitudinal electrostrictive coefficient (Q), the converse piezoelectric constant (d33), and the maximum strain value (Smax%) have changed abnormally around the phase transition temperatures (TR-M and TM-T).

Auger electron spectroscopy analysis for growth interface of cubic boron nitride single crystals synthesized under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Lv, Meizhe; Xu, Bin; Cai, Lichao; Guo, Xiaofei; Yuan, Xingdong

2018-05-01

After rapid cooling, cubic boron nitride (c-BN) single crystals synthesized under high pressure and high temperature (HPHT) are wrapped in the white film powders which are defined as growth interface. In order to make clear that the transition mechanism of c-BN single crystals, the variation of B and N atomic hybrid states in the growth interface is analyzed with the help of auger electron spectroscopy in the Li-based system. It is found that the sp2 fractions of B and N atoms decreases, and their sp3 fractions increases from the outer to the inner in the growth interface. In addition, Lithium nitride (Li3N) are not found in the growth interface by X-ray diffraction (XRD) experiment. It is suggested that lithium boron nitride (Li3BN2) is produced by the reaction of hexagonal boron nitride (h-BN) and Li3N at the first step, and then B and N atoms transform from sp2 into sp3 state with the catalysis of Li3BN2 in c-BN single crystals synthesis process.

Structural and magnetic investigations of single-crystalline neodymium zirconate pyrochlore Nd2Zr2O7

NASA Astrophysics Data System (ADS)

Hatnean, M. Ciomaga; Lees, M. R.; Petrenko, O. A.; Keeble, D. S.; Balakrishnan, G.; Gutmann, M. J.; Klekovkina, V. V.; Malkin, B. Z.

2015-05-01

We report structural and magnetic properties studies of large high-quality single crystals of the frustrated magnet Nd2Zr2O7 . Powder x-ray diffraction analysis confirms that Nd2Zr2O7 adopts the pyrochlore structure. Room-temperature x-ray diffraction and time-of-flight neutron-scattering experiments show that the crystals are stoichiometric in composition with no measurable site disorder. The temperature dependence of the magnetic susceptibility shows no magnetic ordering at temperatures down to 0.5 K. Fits to the magnetic susceptibility data using a Curie-Weiss law reveal a ferromagnetic coupling between the Nd moments. Magnetization versus field measurements show a local Ising anisotropy along the <111 > axes of the Nd3 + ions in the ground state. Specific heat versus temperature measurements in zero applied magnetic field indicate the presence of a thermal anomaly below T ˜7 K, but no evidence of magnetic ordering is observed down to 0.5 K. The experimental temperature dependence of the single-crystal bulk dc susceptibility and isothermal magnetization are analyzed using crystal field theory and the crystal field parameters and exchange coupling constants determined.

Flux growth of Yb(6.6)Ir(6)Sn(16) having mixed-valent ytterbium.

PubMed

Peter, Sebastian C; Subbarao, Udumula; Rayaprol, Sudhindra; Martin, Joshua B; Balasubramanian, Mahalingam; Malliakas, Christos D; Kanatzidis, Mercouri G

2014-07-07

The compound Yb6.6Ir6Sn16 was obtained as single crystals in high yield from the reaction of Yb with Ir and Sn run in excess indium. Single-crystal X-ray diffraction analysis shows that Yb6.6Ir6Sn16 crystallizes in the tetragonal space group P42/nmc with a = b = 9.7105(7) Å and c = 13.7183(11) Å. The crystal structure is composed of a [Ir6Sn16] polyanionic network with cages in which the Yb atoms are embedded. The Yb sublattice features extensive vacancies on one crystallographic site. Magnetic susceptibility measurements on single crystals indicate Curie-Weiss law behavior <100 K with no magnetic ordering down to 2 K. The magnetic moment within the linear region (<100 K) is 3.21 μB/Yb, which is ∼70% of the expected value for a free Yb(3+) ion suggesting the presence of mixed-valent ytterbium atoms. X-ray absorption near edge spectroscopy confirms that Yb6.6Ir6Sn16 exhibits mixed valence. Resistivity and heat capacity measurements for Yb6.6Ir6Sn16 indicate non-Fermi liquid metallic behavior.

The study on the nanomachining property and cutting model of single-crystal sapphire by atomic force microscopy.

PubMed

Huang, Jen-Ching; Weng, Yung-Jin

2014-01-01

This study focused on the nanomachining property and cutting model of single-crystal sapphire during nanomachining. The coated diamond probe is used to as a tool, and the atomic force microscopy (AFM) is as an experimental platform for nanomachining. To understand the effect of normal force on single-crystal sapphire machining, this study tested nano-line machining and nano-rectangular pattern machining at different normal force. In nano-line machining test, the experimental results showed that the normal force increased, the groove depth from nano-line machining also increased. And the trend is logarithmic type. In nano-rectangular pattern machining test, it is found when the normal force increases, the groove depth also increased, but rather the accumulation of small chips. This paper combined the blew by air blower, the cleaning by ultrasonic cleaning machine and using contact mode probe to scan the surface topology after nanomaching, and proposed the "criterion of nanomachining cutting model," in order to determine the cutting model of single-crystal sapphire in the nanomachining is ductile regime cutting model or brittle regime cutting model. After analysis, the single-crystal sapphire substrate is processed in small normal force during nano-linear machining; its cutting modes are ductile regime cutting model. In the nano-rectangular pattern machining, due to the impact of machined zones overlap, the cutting mode is converted into a brittle regime cutting model. © 2014 Wiley Periodicals, Inc.

Theoretical and experimental evaluation of a new organic proton transfer crystal aminoguanidinium p-nitrobenzoate monohydrate for optical limiting applications

NASA Astrophysics Data System (ADS)

Shanmugavadivu, T.; Senthilkumar, K.; Dhandapani, M.; Muthuraja, P.; Balachandar, S.; Sethu Raman, M.

2017-12-01

Aminoguanidinium p-nitrobenzoate monohydrate (AGPNB), an organic third order nonlinear crystal, was successfully grown by the slow evaporation technique. Single crystal XRD analysis reveals that the grown crystal belongs to monoclinic system with P21/n space group. FT-IR, 1H and 13C NMR spectroscopic studies were carried out to confirm the proton transfer. Optical and thermal suitability were assessed by UV-NIR and TG-DTA studies. Hirshfeld surface analysis predicts that the O⋯H/H⋯O interactions dominated over the crystal structure. Third order nonlinearity was studied by Z-scan analysis and it is found that AGPNB can be used as a reverse satuarble absorption (RSA) based optical limiter at 632.8 nm. Computational studies, such as geometry optimization, Natural bond orbital (NBO) analysis, Mulliken population analysis and Molecular electrostatic potential (MEP) were performed at B3LYP/6-311G(d,p) level of theory. The calculated first order hyperpolarizability of AGPNB is found to be 35 times that of urea.

Sulfonamide-containing PTP 1B inhibitors: Docking studies, synthesis and model validation

NASA Astrophysics Data System (ADS)

Niu, Enli; Gan, Qiang; Chen, Xi; Feng, Changgen

2017-01-01

PTP 1B plays an important role in regulating insulin signaling pathway and is regarded as a valid target for curing diabetes and obesity. In this paper, two novel sulfonamide-containing PTP 1B inhibitors were designed, synthesized in mild condition, and characterized by FT-IR, 1H NMR, 13C NMR and elemental analysis. The single crystal of compounds 7 and 8 were obtained and their structures were determined by X-ray single crystal diffraction analysis. In addition, their inhibitory activity were predicted by genetic algorithm, and carried on in vitro enzyme activity test. Of which compound 8 showed good inhibitory activity, in consistent with docking studies.

High pressure single-crystal micro X-ray diffraction analysis with GSE_ADA/RSV software

NASA Astrophysics Data System (ADS)

Dera, Przemyslaw; Zhuravlev, Kirill; Prakapenka, Vitali; Rivers, Mark L.; Finkelstein, Gregory J.; Grubor-Urosevic, Ognjen; Tschauner, Oliver; Clark, Simon M.; Downs, Robert T.

2013-08-01

GSE_ADA/RSV is a free software package for custom analysis of single-crystal micro X-ray diffraction (SCμXRD) data, developed with particular emphasis on data from samples enclosed in diamond anvil cells and subject to high pressure conditions. The package has been in extensive use at the high pressure beamlines of Advanced Photon Source (APS), Argonne National Laboratory and Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. The software is optimized for processing of wide-rotation images and includes a variety of peak intensity corrections and peak filtering features, which are custom-designed to make processing of high pressure SCμXRD easier and more reliable.

Ultratough CVD single crystal diamond and three dimensional growth thereof

DOEpatents

Hemley, Russell J [Washington, DC; Mao, Ho-kwang [Washington, DC; Yan, Chih-shiue [Washington, DC

2009-09-29

The invention relates to a single-crystal diamond grown by microwave plasma chemical vapor deposition that has a toughness of at least about 30 MPa m.sup.1/2. The invention also relates to a method of producing a single-crystal diamond with a toughness of at least about 30 MPa m.sup.1/2. The invention further relates to a process for producing a single crystal CVD diamond in three dimensions on a single crystal diamond substrate.

Development of n- and p-type Doped Perovskite Single Crystals Using Solid-State Single Crystal Growth (SSCG) Technique

DTIC Science & Technology

2017-10-09

doped BaTiO3 single crystal) could be also fabricated by using a BaTiO3 ceramics with the same compositional gradient (Fig. 8). This result has...piezoelectric applications. Compositionally PZT ceramics lie near the MPB between the tetragonal and rhombohedral phases and MPB compositions ...single crystal growth) technique are suitable to grow a variety of “n- and p-type doped” perovskite single crystals of complicated compositions . The

Growth of high quality bulk size single crystals of inverted solubility lithium sulphate monohydrate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Silambarasan, A.; Rajesh, P., E-mail: rajeshp@ssn.edu.in; Ramasamy, P.

2015-06-24

The paper summarizes the processes of growing large lithium sulfate monohydrate (LSMH) single crystals. We have established a procedure to grow high quality bulk size single crystals of inverted solubility LSMH by a newly developed unidirectional crystallization technique called the Sankeranarayenan - Ramasamy (SR) method. The convective flow of crystal growth processes from solution and the conditions of growing crystals of various aspects were discussed. Good quality LSMH single crystal is grown of the size 20 mmX80 mm without cracks, localized-defects and inclusions. The as-grown crystals are suitable for piezoelectric and nonlinear optical applications.

A new method to evaluate the quality of single crystal Cu by an X-ray diffraction butterfly pattern method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu Zhenming; Guo Zhenqi; Li Jianguo

2004-12-15

A new method for the evaluation of the quality of an Ohno continuous cast (OCC) Cu single crystal by X-ray diffraction (XRD) butterfly pattern was brought forward. Experimental results show that the growth direction of single crystal Cu is inclined from both sides of the single crystal Cu rod to the axis and is axially symmetric. The degree of deviation from the [100] orientation from the crystal axis is less than 5 deg. with a casting speed 10-40 mm/min. The orientation of single crystal Cu does not have a fixed direction but is in a regular range. Moreover, the orientationmore » of stray grains in the single crystal Cu is random from continuous casting.« less

Spectral, optical, thermal, Hirshfeld analysis and computational calculations of a new organic proton transfer crystal, 1H-benzo[d][1,2,3]triazol-3-ium-3,5-dinitrobenzoate

NASA Astrophysics Data System (ADS)

Sathya, K.; Dhamodharan, P.; Dhandapani, M.

2018-05-01

A molecular complex, 1H-benzo[d][1,2,3]triazol-3-ium-3,5-dinitrobenzoate, (BTDB), was synthesized, crystallized and characterized by CHN analysis and 1H, 13C NMR spectral studies. The crystal is transparent in entire visible region as evidenced by UV-Vis-NIR spectrum. TG/DTA analysis shows that BTDB is stable up to 150 °C. Single crystal XRD analysis was carried out to ascertain the molecular structure and BTDB crystallizes in the monoclinic system with space group P21/n. Computational studies that include optimization of molecular geometry, natural bond analysis (NBO), Mulliken population analysis and HOMO-LUMO analysis were performed using Gaussian 09 software by B3LYP method at 6-311G(d,p) level. Hirshfeld surfaces and 2D fingerprint plots revealed that O⋯H, H⋯H and O⋯C interactions are the most prevalent. The first order hyperpolarizability (β) of BITB is 44 times greater than urea. The results show that the BTDB may be used for various opto-electronic applications.

Three-Dimensional Stress Fields and Slip Systems for Single Crystal Superalloy Notched Specimens

NASA Technical Reports Server (NTRS)

Magnan, Shannon M.; Throckmorton, David (Technical Monitor)

2002-01-01

Single crystal superalloys have become increasingly popular for turbine blade and vane applications due to their high strength, and creep and fatigue resistance at elevated temperatures. The crystallographic orientation of a single crystal material greatly affects its material properties, including elastic modulus, shear modulus, and ductility. These directional properties, along with the type of loading and temperature, dictate an anisotropic response in the yield strength, creep resistance, creep rupture ductility, fatigue resistance, etc. A significant amount of research has been conducted to determine the material properties in the <001> orientation, yet the material properties deviating from the <001> orientation have not been assessed for all cases. Based on the desired application and design criteria, a crystal orientation is selected to yield the maximum properties. Currently, single crystal manufacturing is able to control the primary crystallographic orientation within 15 of the target orientation, which is an acceptable deviation to meet both performance and cost guidelines; the secondary orientation is rarely specified. A common experiment is the standard load-controlled tensile test, in which specimens with different orientations can be loaded to observe the material response. The deformation behavior of single-crystal materials under tension and compression is known to be a function of not only material orientation, but also of varying microdeformation (i.e. dislocation) mechanisms. The underlying dislocation motion causes deformation via slip, and affects the activation of specific slip systems based on load and orientation. The slip can be analyzed by observing the visible traces left on the surface of the specimen from the slip activity within the single crystal material. The goal of this thesis was to predict the slip systems activated in three-dimensional stress fields of a notched tensile specimen, as a function of crystal orientation, using finite element analysis without addressing microstructural deformation mechanisms that govern their activation. Out of three orientations tested, the specimen with a [110] load orientation and a [001] growth direction had the lowest maximum resolved shear stress; this specimen orientation appears to be the best design candidate for a tensile application.

Spray printing of organic semiconducting single crystals

NASA Astrophysics Data System (ADS)

Rigas, Grigorios-Panagiotis; Payne, Marcia M.; Anthony, John E.; Horton, Peter N.; Castro, Fernando A.; Shkunov, Maxim

2016-11-01

Single-crystal semiconductors have been at the forefront of scientific interest for more than 70 years, serving as the backbone of electronic devices. Inorganic single crystals are typically grown from a melt using time-consuming and energy-intensive processes. Organic semiconductor single crystals, however, can be grown using solution-based methods at room temperature in air, opening up the possibility of large-scale production of inexpensive electronics targeting applications ranging from field-effect transistors and light-emitting diodes to medical X-ray detectors. Here we demonstrate a low-cost, scalable spray-printing process to fabricate high-quality organic single crystals, based on various semiconducting small molecules on virtually any substrate by combining the advantages of antisolvent crystallization and solution shearing. The crystals' size, shape and orientation are controlled by the sheer force generated by the spray droplets' impact onto the antisolvent's surface. This method demonstrates the feasibility of a spray-on single-crystal organic electronics.

Potassium-cobalt sulphate crystal growth assisted by low frequency vibrations

NASA Astrophysics Data System (ADS)

Sadovsky, A.; Ermochenkov, I.; Dubovenko, E.; Sukhanova, E.; Bebyakin, M.; Dubov, V.; Avetissov, I.

2018-02-01

Single crystals of K2Co(SO4)2·6H2O were grown from solution using the temperature reduction method enhanced by the axial low frequency vibration control technique (AVC-technique). Physical modeling of heat-mass transfer in solution under the AVC action was performed. The growth rate of the AVC grown crystal was found to be twice that of the crystal grown under natural convection conditions. Analysis of spectral characteristics (absorption and Raman spectra) as well as structural properties (dislocation density and microhardness) of the grown crystals showed the significant superiority of the AVC technique for the growth of K2Co(SO4)2·6H2O crystals.

Nd Isotope and U-Th-Pb Age Mapping of Single Monazite Grains by Laser Ablation Split Stream Analysis

NASA Astrophysics Data System (ADS)

Fisher, C. M.; Hanchar, J. M.; Miller, C. F.; Phillips, S.; Vervoort, J. D.; Martin, W.

2015-12-01

Monazite is a common accessory mineral that occurs in medium to high grade metamorphic and Ca-poor felsic igneous rocks, and often controls the LREE budget (including Sm and Nd) of the host rock in which it crystallizes. Moreover, it contains appreciable U and Th, making it an ideal mineral for determining U-Th-Pb ages and Sm-Nd isotopic compositions, both of which are readily determined using in situ techniques with very high spatial resolution like LA-MC-ICPMS. Here, we present the results of laser ablation split stream analyses (LASS), which allows for simultaneous determination of the age and initial Nd isotopic composition in a single analysis. Analyses were done using a 20mm laser spot that allowed for detailed Nd isotope mapping of monazite grains (~30 analyses per ~250mm sized grain). Combined with LREE ratios (e.g., Sm/Nd, Ce/Gd, and Eu anomalies) these results yield important petrogenetic constraints on the evolution of peraluminous granites from the Old Woman-Piute batholith in southeastern California. Our findings also allow an improved understanding of the causes of isotope heterogeneity in granitic rocks. U-Th-Pb age mapping across the crystals reveals a single Cretaceous age for all grains with precision and accuracy typical of laser ablation analyses (~2%). In contrast, the concurrent Nd isotope mapping yields homogeneous initial Nd isotope compositions for some grains and large initial intra-grain variations of up to 8 epsilon units in others. The grains that yield homogeneous Nd isotope compositions have REE ratios suggesting that they crystallized in a fractionally crystallizing magma. Conversely, other grains, which also record fractional crystallization of both feldspar and LREE rich minerals, demonstrate a change in the Nd isotope composition of the magma during crystallization of monazite. Comparison of inter- and intra-grain Nd isotope compositions reveals further details on the potential mechanisms responsible for isotope heterogeneity present in single rock samples. This method highlights the potential of single grain isotope mapping of LREE phases such as monazite, allanite, and titanite for understanding both igneous and metamorphic petrogenesis.

Gallium arsenide single crystal solar cell structure and method of making

NASA Technical Reports Server (NTRS)

Stirn, Richard J. (Inventor)

1983-01-01

A production method and structure for a thin-film GaAs crystal for a solar cell on a single-crystal silicon substrate (10) comprising the steps of growing a single-crystal interlayer (12) of material having a closer match in lattice and thermal expansion with single-crystal GaAs than the single-crystal silicon of the substrate, and epitaxially growing a single-crystal film (14) on the interlayer. The material of the interlayer may be germanium or graded germanium-silicon alloy, with low germanium content at the silicon substrate interface, and high germanium content at the upper surface. The surface of the interface layer (12) is annealed for recrystallization by a pulsed beam of energy (laser or electron) prior to growing the interlayer. The solar cell structure may be grown as a single-crystal n.sup.+ /p shallow homojunction film or as a p/n or n/p junction film. A Ga(Al)AS heteroface film may be grown over the GaAs film.

Preparation of fine single crystals of magnetic superconductor RuSr2GdCu2O8-δ by partial melting

NASA Astrophysics Data System (ADS)

Yamaki, Kazuhiro; Bamba, Yoshihiro; Irie, Akinobu

2018-03-01

In this study, fine uniform RuSr2GdCu2O8-δ (RuGd-1212) single crystals have been successfully prepared by partial melting. Synthesis temperature could be lowered to a value not exceeding the decomposition temperature of RuGd-1212 using the Sr-Gd-Cu-O flux. The crystals grown by alumina boats are cubic, which coincides with the result of a previous study of RuGd-1212 single crystals using platinum crucibles. The single crystals were up to 15 × 15 × 15 µm3 in size and their lattice constants were consistent with those of polycrystalline samples reported previously. Although the present size of single crystals is not sufficient for measurements, the partial melting technique will be beneficial for future progress of research using RuGd-1212 single crystals. Appropriate nominal composition, sintering atmosphere, and temperature are essential factors for growing RuGd-1212 single crystals.

Space-based solar power conversion and delivery systems study. Volume 4: Energy conversion systems studies

NASA Technical Reports Server (NTRS)

1977-01-01

Solar cells and optical configurations for the SSPS were examined. In this task, three specific solar cell materials were examined: single crystal silicon, single crystal gallium arsenide, and polycrystalline cadmium sulfide. The comparison of the three different cells on the basis of a subsystem parametric cost per kW of SSPS-generated power at the terrestrial utility interface showed that gallium arsenide was the most promising solar cell material at high concentration ratios. The most promising solar cell material with no concentration, was dependent upon the particular combination of parameters representing cost, mass and performance that were chosen to represent each cell in this deterministic comparative analysis. The potential for mass production, based on the projections of the present state-of-the-art would tend to favor cadmium sulfide in lieu of single crystal silicon or gallium arsenide solar cells.

A crystallographic model for nickel base single crystal alloys

NASA Technical Reports Server (NTRS)

Dame, L. T.; Stouffer, D. C.

1988-01-01

The purpose of this research is to develop a tool for the mechanical analysis of nickel-base single-crystal superalloys, specifically Rene N4, used in gas turbine engine components. This objective is achieved by developing a rate-dependent anisotropic constitutive model and implementing it in a nonlinear three-dimensional finite-element code. The constitutive model is developed from metallurgical concepts utilizing a crystallographic approach. An extension of Schmid's law is combined with the Bodner-Partom equations to model the inelastic tension/compression asymmetry and orientation-dependence in octahedral slip. Schmid's law is used to approximate the inelastic response of the material in cube slip. The constitutive equations model the tensile behavior, creep response and strain-rate sensitivity of the single-crystal superalloys. Methods for deriving the material constants from standard tests are also discussed. The model is implemented in a finite-element code, and the computed and experimental results are compared for several orientations and loading conditions.

Demonstration of single crystal growth via solid-solid transformation of a glass

DOE PAGES

Savytskii, Dmytro; Knorr, Brian; Dierolf, Volkmar; ...

2016-03-18

Many advanced technologies have relied on the availability of single crystals of appropriate material such as silicon for microelectronics or superalloys for turbine blades. Similarly, many promising materials could unleash their full potential if they were available in a single crystal form. However, the current methods are unsuitable for growing single crystals of these oftentimes incongruently melting, unstable or metastable materials. Here we demonstrate a strategy to overcome this hurdle by avoiding the gaseous or liquid phase, and directly converting glass into a single crystal. Specifically, Sb 2S 3 single crystals are grown in Sb-S-I glasses as an example ofmore » this approach. In this first unambiguous demonstration of an all-solid-state glass → crystal transformation, extraneous nucleation is avoided relative to crystal growth via spatially localized laser heating and inclusion of a suitable glass former in the composition. Lastly, the ability to fabricate patterned single-crystal architecture on a glass surface is demonstrated, providing a new class of micro-structured substrate for low cost epitaxial growth, active planar devices, etc.« less

Study of single crystals of metal solid solutions

NASA Technical Reports Server (NTRS)

Doty, J. P.; Reising, J. A.

1973-01-01

The growth of single crystals of relatively high melting point metals such as silver, copper, gold, and their alloys was investigated. The purpose was to develop background information necessary to support a space flight experiment and to generate ground based data for comparison. The ground based data, when compared to the data from space grown crystals, are intended to identify any effects which zero-gravity might have on the basic process of single crystal growth of these metals. The ultimate purposes of the complete investigation are to: (1) determine specific metals and alloys to be investigated; (2) grow single metal crystals in a terrestrial laboratory; (3) determine crystal characteristics, properties, and growth parameters that will be effected by zero-gravity; (4) evaluate terrestrially grown crystals; (5) grow single metal crystals in a space laboratory such as Skylab; (6) evaluate the space grown crystals; (7) compare for zero-gravity effects of crystal characteristics, properties, and parameters; and (8) make a recommendation as to production of these crystals as a routine space manufacturing proceses.

Crystal growth and scintillation properties of Pr-doped SrI2 single crystals

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Ito, Tomoki; Yoshino, Masao; Yamaji, Akihiro; Ohashi, Yuji; Kurosawa, Shunsuke; Kamada, Kei; Yoshikawa, Akira

2018-04-01

Pr-doped SrI2 (Pr:SrI2) single crystals with various Pr concentrations were grown by the halide-micro-pulling-down (H-μ-PD) method, and the scintillation properties were investigated. Pr1%:SrI2 single crystal with high transparency could be grown by the H-μ-PD method while Pr2, 3 and 5%:SrI2 single crystals included some cracks and opaque parts. In the photoluminescence spectrum of the Pr1%:SrI2 single crystal, an emission peak originated from the Pr3+ ion was observed around 435 nm while the radioluminescence spectra showed an emission peak around 535 nm for the undoped SrI2 and Pr:SrI2 single crystals. Light yields of Pr1, 2, 3 and 5%:SrI2 single crystals under γ-ray irradiation were 7700, 8700, 7200 and 6700 photons/MeV, respectively. Decay times of Pr1 and 2%:SrI2 single crystals under γ-ray irradiation were 55.9 and 35.0 ns of the fast decay component, and 435 and 408 ns of the slow decay component, respectively.

Cationic metal complex, carbonatobis(1,10-phenanthroline)cobalt(III) as anion receptor: Synthesis, characterization, single crystal X-ray structure and packing analysis of [Co(phen) 2CO 3](3,5-dinitrobenzoate)·5H 2O

NASA Astrophysics Data System (ADS)

Sharma, Raj Pal; Singh, Ajnesh; Brandão, Paula; Felix, Vitor; Venugopalan, Paloth

2009-03-01

To explore the potential of [Co(phen) 2CO 3] + as anion receptor, red coloured single crystals of [Co(phen) 2CO 3](dnb)·5H 2O (dnb = 3,5-dinitrobenzoate) were obtained by recrystallizing the red microcrystalline product synthesised by the reaction of carbonatobis (1,10-phenanthroline)cobalt(III)chloride with sodium salt of 3,5-dinitrobenzoic acid in aqueous medium (1:1 molar ratio). The newly synthesized complex salt has been characterized by elemental analysis, spectroscopic studies (IR, UV/visible, 1H and 13C NMR), solubility and conductance measurements. The complex salt crystallizes in the triclinic crystal system with space group P1¯, having the cell dimensions a = 10.3140(8), b = 12.2885(11), c = 12.8747(13), α = 82.095(4), β = 85.617(4), γ = 79.221(4)°, V = 1585.6(2) Å 3, Z = 2. Single crystal X-ray structure determination revealed ionic structure consisting of cationic carbonatobis(1,10-phenanthroline)cobalt(III), dnb anion and five lattice water molecule. In the complex cation [Co(phen) 2CO 3] +, the cobalt(III) is bonded to four nitrogen atoms, originating from two phenanthroline ligands and two oxygen atoms from the bidentate carbonato group showing an octahedral geometry around cobalt(III) center. Supramolecular networks between ionic groups [ CHphen+⋯Xanion-] by second sphere coordination i.e. C sbnd H⋯O (benzoate), C sbnd H⋯O (nitro), C sbnd H⋯O (water) besides electrostatic forces of attraction alongwith π-π interactions stabilize the crystal lattice.

Serial snapshot crystallography for materials science with SwissFEL

DOE PAGES

Dejoie, Catherine; Smeets, Stef; Baerlocher, Christian; ...

2015-04-21

New opportunities for studying (sub)microcrystalline materials with small unit cells, both organic and inorganic, will open up when the X-ray free electron laser (XFEL) presently being constructed in Switzerland (SwissFEL) comes online in 2017. Our synchrotron-based experiments mimicking the 4%-energy-bandpass mode of the SwissFEL beam show that it will be possible to record a diffraction pattern of up to 10 randomly oriented crystals in a single snapshot, to index the resulting reflections, and to extract their intensities reliably. The crystals are destroyed with each XFEL pulse, but by combining snapshots from several sets of crystals, a complete set of datamore » can be assembled, and crystal structures of materials that are difficult to analyze otherwise will become accessible. Even with a single shot, at least a partial analysis of the crystal structure will be possible, and with 10–50 femtosecond pulses, this offers tantalizing possibilities for time-resolved studies.« less

Inverse Slip Accompanying Twinning and Detwinning during Cyclic Loading of Magnesium Single Crystal

DOE PAGES

Yu, Qin; Wang, Jian; Jiang, Yanyao

2013-01-01

In situ , observation of twinning and detwinning in magnesium single crystals during tension-compression cyclic loading was made using optical microscopy. A quantitative analysis of plastic strain indicates that twinning and detwinning experience two stages, low and high work hardening de-twinning, and pure re-twinning and fresh twinning combined with retwinning. Slip is always activated. For the first time, inverse slip accompanying with pure retwinning and high work hardening detwinning was experimentally identified, which provides insights in better understanding of the activity of twining, detwinning, and slips.

Custom Coordination Environments for Lanthanoids: Tripodal Ligands Achieve Near-Perfect Octahedral Coordination for Two Dysprosium-Based Molecular Nanomagnets.

PubMed

Lim, Kwang Soo; Baldoví, José J; Jiang, ShangDa; Koo, Bong Ho; Kang, Dong Won; Lee, Woo Ram; Koh, Eui Kwan; Gaita-Ariño, Alejandro; Coronado, Eugenio; Slota, Michael; Bogani, Lapo; Hong, Chang Seop

2017-05-01

Controlling the coordination sphere of lanthanoid complexes is a challenging critical step toward controlling their relaxation properties. Here we present the synthesis of hexacoordinated dysprosium single-molecule magnets, where tripodal ligands achieve a near-perfect octahedral coordination. We perform a complete experimental and theoretical investigation of their magnetic properties, including a full single-crystal magnetic anisotropy analysis. The combination of electrostatic and crystal-field computational tools (SIMPRE and CONDON codes) allows us to explain the static behavior of these systems in detail.

The gamut of alkoxy radicals

NASA Astrophysics Data System (ADS)

Box, Harold C.; Budzinski, Edwin E.; Freund, Harold G.

1984-12-01

It is shown that various radicals exhibiting diverse ESR and ENDOR spectral characteristics are nonetheless a closely related family of alkoxy radicals. The relationship is established by correlating the g tensor with crystal structure and by relating dihedral angles inferred from proton hyperfine couplings to dihedral angles inferred from the g tensor and crystal structure. The analysis also serves to demonstrate that an ESR absorption observed in x-irradiated single crystals of uridine 5'-monophosphate is due to an alkoxy radical.

Subsurface Stress Fields in FCC Single Crystal Anisotropic Contacts

NASA Technical Reports Server (NTRS)

Arakere, Nagaraj K.; Knudsen, Erik; Swanson, Gregory R.; Duke, Gregory; Ham-Battista, Gilda

2004-01-01

Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and alternating stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent high cycle fatigue (HCF) failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and non-crystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. This paper presents analytical and numerical techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts. The subsurface stress results are required for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades. An analytical procedure is presented for evaluating the subsurface stresses in the elastic half-space, based on the adaptation of a stress function method outlined by Lekhnitskii. Numerical results are presented for cylindrical and spherical anisotropic contacts, using finite element analysis (FEA). Effects of crystal orientation on stress response and fatigue life are examined. Obtaining accurate subsurface stress results for anisotropic single crystal contact problems require extremely refined three-dimensional (3-D) finite element grids, especially in the edge of contact region. Obtaining resolved shear stresses (RSS) on the principal slip planes also involves considerable post-processing work. For these reasons it is very advantageous to develop analytical solution schemes for subsurface stresses, whenever possible.

Structure analysis on synthetic emerald crystals

NASA Astrophysics Data System (ADS)

Lee, Pei-Lun; Lee, Jiann-Shing; Huang, Eugene; Liao, Ju-Hsiou

2013-05-01

Single crystals of emerald synthesized by means of the flux method were adopted for crystallographic analyses. Emerald crystals with a wide range of Cr3+-doping content up to 3.16 wt% Cr2O3 were examined by X-ray single crystal diffraction refinement method. The crystal structures of the emerald crystals were refined to R 1 (all data) of 0.019-0.024 and w R 2 (all data) of 0.061-0.073. When Cr3+ substitutes for Al3+, the main adjustment takes place in the Al-octahedron and Be-tetrahedron. The effect of substitution of Cr3+ for Al3+ in the beryl structure results in progressively lengthening of the Al-O distance, while the length of the other bonds remains nearly unchanged. The substitution of Cr3+ for Al3+ may have caused the expansion of a axis, while keeping the c axis unchanged in the emerald lattice. As a consequence, the Al-O-Si and Al-O-Be bonding angles are found to decrease, while the angle of Si-O-Be increases as the Al-O distance increases during the Cr replacement.

Vibrational and structural investigation of SOUL protein single crystals by using micro-Raman spectroscopy

NASA Astrophysics Data System (ADS)

Rossi, Barbara; Giarola, Marco; Mariotto, Gino; Ambrosi, Emmanuele; Monaco, Hugo L.

2010-05-01

Protein SOUL is a new member of the recently discovered putative heme-binding protein family called SOUL/HEBP and, to date, no structural information exists for this protein. Here, micro-Raman spectroscopy is used to study the vibrational properties of single crystals obtained from recombinant protein SOUL by means of two different optimization routes. This spectroscopic approach offers the valuable advantage of the in-situ collection of experimental data from protein crystals, placed onto a hanging-drop plate, under the same conditions used to grow the crystals. By focusing on the regions of amides I and III bands, some secondary structure characteristic features have been recognized. Moreover, some side-chain marker bands were observed in the Raman spectra of SOUL crystals and the unambiguous assignment of these peaks inferred by comparing the experimental Raman spectra of pure amino acids and their Raman intensities computed using quantum chemical calculations. Our comparative analysis allows to get a deeper understanding of the side-chain environments and of the interactions involving these specific amino acids in the two different SOUL crystals.

Prediction and theoretical characterization of p-type organic semiconductor crystals for field-effect transistor applications.

PubMed

Atahan-Evrenk, Sule; Aspuru-Guzik, Alán

2014-01-01

The theoretical prediction and characterization of the solid-state structure of organic semiconductors has tremendous potential for the discovery of new high performance materials. To date, the theoretical analysis mostly relied on the availability of crystal structures obtained through X-ray diffraction. However, the theoretical prediction of the crystal structures of organic semiconductor molecules remains a challenge. This review highlights some of the recent advances in the determination of structure-property relationships of the known organic semiconductor single-crystals and summarizes a few available studies on the prediction of the crystal structures of p-type organic semiconductors for transistor applications.

Improved ferroelectric and pyroelectric parameters in iminodiacetic acid doped TGS crystal

NASA Astrophysics Data System (ADS)

Rai, Chitharanjan; Sreenivas, K.; Dharmaprakash, S. M.

2010-01-01

Single crystals of Iminodiacetic acid (HN(CH 2COOH) 2) doped Triglycine sulphate (IDATGS) has been grown from aqueous solution at constant temperature by slow evaporation technique. The concentration of the dopant in the TGS solution was 2 mol%. The X-ray diffraction analysis indicates that there is significant change in the lattice parameters compared to pure TGS crystal. The IDATGS crystal has larger transition temperature and observed higher and uniform figure of merit over most part of the ferroelectric phase. These crystals also exhibit higher internal bias field and micro-hardness number compared to pure TGS. Therefore IDATGS may be a potential material for IR detectors.

Numerical study of slip system activity and crystal lattice rotation under wedge nanoindents in tungsten single crystals

NASA Astrophysics Data System (ADS)

Volz, T.; Schwaiger, R.; Wang, J.; Weygand, S. M.

2018-05-01

Tungsten is a promising material for plasma facing components in future nuclear fusion reactors. In the present work, we numerically investigate the deformation behavior of unirradiated tungsten (a body-centered cubic (bcc) single crystal) underneath nanoindents. A finite element (FE) model is presented to simulate wedge indentation. Crystal plasticity finite element (CPFE) simulations were performed for face-centered and body-centered single crystals accounting for the slip system family {110} <111> in the bcc crystal system and the {111} <110> slip family in the fcc system. The 90° wedge indenter was aligned parallel to the [1 ¯01 ]-direction and indented the crystal in the [0 1 ¯0 ]-direction up to a maximum indentation depth of 2 µm. In both, the fcc and bcc single crystals, the activity of slip systems was investigated and compared. Good agreement with the results from former investigations on fcc single crystals was observed. Furthermore, the in-plane lattice rotation in the material underneath an indent was determined and compared for the fcc and bcc single crystals.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Astrophysics Data System (ADS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-09-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-01-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

Mechanochemical Synthesis of Carbon Nanothread Single Crystals.

PubMed

Li, Xiang; Baldini, Maria; Wang, Tao; Chen, Bo; Xu, En-Shi; Vermilyea, Brian; Crespi, Vincent H; Hoffmann, Roald; Molaison, Jamie J; Tulk, Christopher A; Guthrie, Malcolm; Sinogeikin, Stanislav; Badding, John V

2017-11-15

Synthesis of well-ordered reduced dimensional carbon solids with extended bonding remains a challenge. For example, few single-crystal organic monomers react under topochemical control to produce single-crystal extended solids. We report a mechanochemical synthesis in which slow compression at room temperature under uniaxial stress can convert polycrystalline or single-crystal benzene monomer into single-crystalline packings of carbon nanothreads, a one-dimensional sp 3 carbon nanomaterial. The long-range order over hundreds of microns of these crystals allows them to readily exfoliate into fibers. The mechanochemical reaction produces macroscopic single crystals despite large dimensional changes caused by the formation of multiple strong, covalent C-C bonds to each monomer and a lack of reactant single-crystal order. Therefore, it appears not to follow a topochemical pathway, but rather one guided by uniaxial stress, to which the nanothreads consistently align. Slow-compression room-temperature synthesis may allow diverse molecular monomers to form single-crystalline packings of polymers, threads, and higher dimensional carbon networks.

The timing resolution of scintillation-detector systems: Monte Carlo analysis

NASA Astrophysics Data System (ADS)

Choong, Woon-Seng

2009-11-01

Recent advancements in fast scintillating materials and fast photomultiplier tubes (PMTs) have stimulated renewed interest in time-of-flight (TOF) positron emission tomography (PET). It is well known that the improvement in the timing resolution in PET can significantly reduce the noise variance in the reconstructed image resulting in improved image quality. In order to evaluate the timing performance of scintillation detectors used in TOF PET, we use Monte Carlo analysis to model the physical processes (crystal geometry, crystal surface finish, scintillator rise time, scintillator decay time, photoelectron yield, PMT transit time spread, PMT single-electron response, amplifier response and time pick-off method) that can contribute to the timing resolution of scintillation-detector systems. In the Monte Carlo analysis, the photoelectron emissions are modeled by a rate function, which is used to generate the photoelectron time points. The rate function, which is simulated using Geant4, represents the combined intrinsic light emissions of the scintillator and the subsequent light transport through the crystal. The PMT output signal is determined by the superposition of the PMT single-electron response resulting from the photoelectron emissions. The transit time spread and the single-electron gain variation of the PMT are modeled in the analysis. Three practical time pick-off methods are considered in the analysis. Statistically, the best timing resolution is achieved with the first photoelectron timing. The calculated timing resolution suggests that a leading edge discriminator gives better timing performance than a constant fraction discriminator and produces comparable results when a two-threshold or three-threshold discriminator is used. For a typical PMT, the effect of detector noise on the timing resolution is negligible. The calculated timing resolution is found to improve with increasing mean photoelectron yield, decreasing scintillator decay time and decreasing transit time spread. However, only substantial improvement in the timing resolution is obtained with improved transit time spread if the first photoelectron timing is less than the transit time spread. While the calculated timing performance does not seem to be affected by the pixel size of the crystal, it improves for an etched crystal compared to a polished crystal. In addition, the calculated timing resolution degrades with increasing crystal length. These observations can be explained by studying the initial photoelectron rate. Experimental measurements provide reasonably good agreement with the calculated timing resolution. The Monte Carlo analysis developed in this work will allow us to optimize the scintillation detectors for timing and to understand the physical factors limiting their performance.

The timing resolution of scintillation-detector systems: Monte Carlo analysis.

PubMed

Choong, Woon-Seng

2009-11-07

Recent advancements in fast scintillating materials and fast photomultiplier tubes (PMTs) have stimulated renewed interest in time-of-flight (TOF) positron emission tomography (PET). It is well known that the improvement in the timing resolution in PET can significantly reduce the noise variance in the reconstructed image resulting in improved image quality. In order to evaluate the timing performance of scintillation detectors used in TOF PET, we use Monte Carlo analysis to model the physical processes (crystal geometry, crystal surface finish, scintillator rise time, scintillator decay time, photoelectron yield, PMT transit time spread, PMT single-electron response, amplifier response and time pick-off method) that can contribute to the timing resolution of scintillation-detector systems. In the Monte Carlo analysis, the photoelectron emissions are modeled by a rate function, which is used to generate the photoelectron time points. The rate function, which is simulated using Geant4, represents the combined intrinsic light emissions of the scintillator and the subsequent light transport through the crystal. The PMT output signal is determined by the superposition of the PMT single-electron response resulting from the photoelectron emissions. The transit time spread and the single-electron gain variation of the PMT are modeled in the analysis. Three practical time pick-off methods are considered in the analysis. Statistically, the best timing resolution is achieved with the first photoelectron timing. The calculated timing resolution suggests that a leading edge discriminator gives better timing performance than a constant fraction discriminator and produces comparable results when a two-threshold or three-threshold discriminator is used. For a typical PMT, the effect of detector noise on the timing resolution is negligible. The calculated timing resolution is found to improve with increasing mean photoelectron yield, decreasing scintillator decay time and decreasing transit time spread. However, only substantial improvement in the timing resolution is obtained with improved transit time spread if the first photoelectron timing is less than the transit time spread. While the calculated timing performance does not seem to be affected by the pixel size of the crystal, it improves for an etched crystal compared to a polished crystal. In addition, the calculated timing resolution degrades with increasing crystal length. These observations can be explained by studying the initial photoelectron rate. Experimental measurements provide reasonably good agreement with the calculated timing resolution. The Monte Carlo analysis developed in this work will allow us to optimize the scintillation detectors for timing and to understand the physical factors limiting their performance.

High-resolution EPMA X-ray images of mother liquid inclusions in a Pd2Ga single crystal

NASA Astrophysics Data System (ADS)

Müller, D.; Schwerin, J.; Gille, P.; Fehr, K. T.

2014-03-01

During crystal growth from solution inclusions of different compositions were trapped at the rim of a Pd2Ga single crystal. Their fine-grained (< 5 μm) internal structure demands special requirements for electron microprobe analysis, realized by low-voltage (5 keV) element mapping applying a step size of 0.138 μm for each pixel. It can be shown, that these inclusions represent an isolated chemical system, and that crystallisation upon cooling follows the expected thermodynamic phase relations. Thus the final composition in the centre of the inclusion consists of a small-scale mixture of PdGa and Pd5Ga3 evolved out of a solid-solid decomposition of Pd5Ga4.

Crystal engineering: co-crystals of cinnamic acid derivatives with a pyridyl derivative co-crystallizer.

PubMed

Lorenzo, Daniel A; Forrest, Sebastian J K; Sparkes, Hazel A

2016-02-01

A number of hydrogen-bonded co-crystals, consisting of a cinnamic acid derivative and a pyridyl co-crystallizer, have been synthesized and their properties investigated by X-ray diffraction. Samples were prepared by recrystallization or solvent drop grinding of trans-cinnamic acid (1), 4-methylcinnamic acid (2), 4-methoxy cinnamic acid (3) or 3,4-methoxy cinnamic acid (4), with 4,4-dipyridyl (A), iso-nicotinamide (B) or nicotinamide (C). The X-ray single-crystal structures of seven novel co-crystals, obtained through recrystallization, are examined and the hydrogen-bonding interactions discussed. Consistent hydrogen-bonding motifs were observed for samples prepared when using 4,4-dipyridyl (A) or iso-nicotinamide (B) as the co-crystallizing agent. Powder X-ray diffraction analysis of the samples prepared by solvent drop grinding suggests the formation of ten co-crystals.

Crystal growth and scintillation properties of Nd-doped Lu 3Al 5O 12 single crystals with different Nd concentrations

NASA Astrophysics Data System (ADS)

Sugiyama, Makoto; Fujimoto, Yutaka; Yanagida, Takayuki; Yokota, Yuui; Pejchal, Jan; Furuya, Yuki; Tanaka, Hidehiko; Yoshikawa, Akira

2011-04-01

Nd 0.1%, 0.5%, 1% and 3% doped Lu 3Al 5O 12 (Nd:LuAG) single crystals were grown in the nitrogen atmosphere by the micro-pulling down (μ-PD) method. The grown crystals had a single-phase confirmed by powder XRD analysis. In absorption spectra, some weak absorption lines due to Nd 3+ 4f-4f transitions were observed and their intensity increased with the increase of Nd concentration. When excited by 241Am α-ray, a broad emission peak due to defects in the host lattice at 320 nm and some sharp lines due to Nd 3+ 4f-4f transitions at wavelength longer than 400 nm were observed. The decay time profiles of Nd:LuAG under γ-ray excitation were well approximated by two exponential function of 340-760 ns and 3-5 μs for each sample. By pulse height measurement using 137Cs, Nd 0.5%:LuAG showed the highest light yield of 7600 ± 760 photons/MeV.

Microstructure and pinning properties of hexagonal-disc shaped single crystalline MgB2

NASA Astrophysics Data System (ADS)

Jung, C. U.; Kim, J. Y.; Chowdhury, P.; Kim, Kijoon H.; Lee, Sung-Ik; Koh, D. S.; Tamura, N.; Caldwell, W. A.; Patel, J. R.

2002-11-01

We synthesized hexagonal-disc-shaped MgB2 single crystals under high-pressure conditions and analyzed the microstructure and pinning properties. The lattice constants and the Laue pattern of the crystals from x-ray micro-diffraction showed the crystal symmetry of MgB2. A thorough crystallographic mapping within a single crystal showed that the edge and c axis of hexagonal-disc shape exactly matched the [101¯0] and the [0001] directions of the MgB2 phase. Thus, these well-shaped single crystals may be the best candidates for studying the direction dependences of the physical properties. The magnetization curve and the magnetic hysteresis curve for these single crystals showed the existence of a wide reversible region and weak pinning properties, which supported our single crystals being very clean.

Diffusion of CO2 in Large Crystals of Cu-BTC MOF.

PubMed

Tovar, Trenton M; Zhao, Junjie; Nunn, William T; Barton, Heather F; Peterson, Gregory W; Parsons, Gregory N; LeVan, M Douglas

2016-09-14

Carbon dioxide adsorption in metal-organic frameworks has been widely studied for applications in carbon capture and sequestration. A critical component that has been largely overlooked is the measurement of diffusion rates. This paper describes a new reproducible procedure to synthesize millimeter-scale Cu-BTC single crystals using concentrated reactants and an acetic acid modulator. Microscopic images, X-ray diffraction patterns, Brunauer-Emmett-Teller surface areas, and thermogravimetric analysis results all confirm the high quality of these Cu-BTC single crystals. The large crystal size aids in the accurate measurement of micropore diffusion coefficients. Concentration-swing frequency response performed at varying gas-phase concentrations gives diffusion coefficients that show very little dependence on the loading up to pressures of 0.1 bar. The measured micropore diffusion coefficient for CO2 in Cu-BTC is 1.7 × 10(-9) m(2)/s.

Controlled vapor crystal growth of N a4I r3O8 : A three-dimensional quantum spin liquid candidate

NASA Astrophysics Data System (ADS)

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; Ren, Yang; Chen, Yu-Sheng; Dally, Rebecca; Wilson, Stephen D.; Islam, Zahirul; Mitchell, J. F.

2018-04-01

We report the successful bulk single-crystal growth of the hyperkagome lattice iridate N a4I r3O8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q =(1 /3 ,1 /3 ,1 /3 ) based on the cubic substructure with cell parameter a =8.986 (1 )Å . This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ions at the notionally disordered Na sites as a plausible origin for the observed superlattice.

Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

DOE PAGES

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; ...

2018-04-24

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

Study of ceramic products and processing techniques in space. [using computerized simulation

NASA Technical Reports Server (NTRS)

Markworth, A. J.; Oldfield, W.

1974-01-01

An analysis of the solidification kinetics of beta alumina in a zero-gravity environment was carried out, using computer-simulation techniques, in order to assess the feasibility of producing high-quality single crystals of this material in space. The two coupled transport processes included were movement of the solid-liquid interface and diffusion of sodium atoms in the melt. Results of the simulation indicate that appreciable crystal-growth rates can be attained in space. Considerations were also made of the advantages offered by high-quality single crystals of beta alumina for use as a solid electrolyte; these clearly indicate that space-grown materials are superior in many respects to analogous terrestrially-grown crystals. Likewise, economic considerations, based on the rapidly expanding technological applications for beta alumina and related fast ionic conductors, reveal that the many superior qualities of space-grown material justify the added expense and experimental detail associated with space processing.

Double layer zinc-UDP coordination polymers: structure and properties.

PubMed

Qiu, Qi-Ming; Gu, Leilei; Ma, Hongwei; Yan, Li; Liu, Minghua; Li, Hui

2018-05-17

A homochiral Zn-UDP coordination polymer with an alternating parallel ABAB sequence was constructed and studied by X-ray single crystal diffraction analysis. Its crystal structure shows that there are potentially open sites in the 2D layers. The activation of the sites makes the coordination polymer a fluorescent sensor for novel heterogeneous detection of amino acids.

Method for the preparation of inorganic single crystal and polycrystalline electronic materials

NASA Technical Reports Server (NTRS)

Groves, W. O. (Inventor)

1969-01-01

Large area, semiconductor crystals selected from group 3-5 compounds and alloys are provided for semiconductor device fabrication by the use of a selective etching operation which completely removes the substrate on which the desired crystal was deposited. The substrate, selected from the same group as the single crystal, has a higher solution rate than the epitaxial single crystal which is essentially unaffected by the etching solution. The preparation of gallium phosphide single crystals using a gallium arsenide substrate and a concentrated nitric acid etching solution is described.

Optical, Fluorescence with quantum analysis of hydrazine (1, 3- Dinitro Phenyl) by DFT and Ab initio approach

NASA Astrophysics Data System (ADS)

Cecily Mary Glory, D.; Sambathkumar, K.; Madivanane, R.; Velmurugan, G.; Gayathri, R.; Nithiyanantham, S.; Venkatachalapathy, M.; Rajkamal, N.

2018-07-01

Experimental and computational study of molecular structure, vibrational and UV-spectral analysis of Hydrazine (1, 3- Dinitrophenyl) (HDP) derivatives. The crystal was grown by slow cooling method and the crystalline perfection of single crystals was evaluated by high resolution X-ray diffractometry (HRXRD) using a multicrystal X-ray diffractometer. Fluorescence, FT-IR and FT-Raman spectra of HDP crystal were recorded. The assignments of the vibrational spectra have been carried out with the help of normal co-ordinate analysis (NCA) followed by scaled quantum force field methodology (SQMFF). NMR studies have confirmed respectively the crystal structure and functional groups of the grown crystal. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) result complements the experimental findings. The calculated MESP, UV, HOMO-LUMO energies show that charge transfer done within the molecule. And various thermodynamic parameters are studied. Fukui determines the local reactive site of electrophilic, nucleophilic, descriptor.

A combined experimental and in silico characterization to highlight additional structural features and properties of a potentially new drug

NASA Astrophysics Data System (ADS)

Bastos, Isadora T. S.; Costa, Fanny N.; Silva, Tiago F.; Barreiro, Eliezer J.; Lima, Lídia M.; Braz, Delson; Lombardo, Giuseppe M.; Punzo, Francesco; Ferreira, Fabio F.; Barroso, Regina C.

2017-10-01

LASSBio-1755 is a new cycloalkyl-N-acylhydrazone parent compound designed for the development of derivatives with antinociceptive and anti-inflammatory activities. Although single crystal X-ray diffraction has been considered as the golden standard in structure determination, we successfully used X-ray powder diffraction data in the structural determination of new synthesized compounds, in order to overcome the bottle-neck due to the difficulties experienced in harvesting good quality single crystals of the compounds. We therefore unequivocally assigned the relative configuration (E) to the imine double bond and a s-cis conformation of the amide function of the N-acylhydrazone compound. These features are confirmed by a computational analysis performed on the basis of molecular dynamics calculations, which are extended not only to the structural characteristics but also to the analysis of the anisotropic atomic displacement parameters, a further information - missed in a typical powder diffraction analysis. The so inferred data were used to perform additional cycles of refinement and eventually generate a new cif file with additional physical information. Furthermore, crystal morphology prediction was performed, which is in agreement with the experimental images acquired by scanning electron microscopy, thus providing useful information on possible alternative paths for better crystallization strategies.

Physico-chemical characterization, density functional theory (DFT) studies and Hirshfeld surface analysis of a new organic optical material: 1H-benzo[d]imidazol-3-ium-2,4,6-trinitrobenzene-1,3 bis(olate)

NASA Astrophysics Data System (ADS)

Dhamodharan, P.; Sathya, K.; Dhandapani, M.

2017-10-01

A novel organic crystal, 1H-benzo[d]imidazol-3-ium-2,4,6-trinitrobenzene-1,3 bis(olate) (BITB), was synthesized. Single crystals of BITB were harvested by solution growth-slow evaporation technique. 1H and 13C NMR spectroscopic techniques were utilized to confirm the presence of various types of carbons and protons in BITB. Single crystal XRD confirms that BITB crystallizes in monoclinic system with a space group of P21/n. The suitability of this material for optical applications was assessed by optical absorption, transmittance, reflectance and refractive index spectroscopic techniques. Gaussian 09 program at B3LYP/6-311++G(d,p) level of basis set as used for the optimization of molecular structure of BITB. Greater first order hyperpolarizability value of BITB is due to intensive hydrogen bond network in the crystal. The value is 15 times greater than that of Urea, a reference standard. Computation of frontier molecular orbitals and electrostatic potential surface helped to understand the electron density and reactive sites in BITB. The material was thermally stable up to 220 °C. Hirshfeld surface analysis was performed to quantify the covalent and non covalent interactions.

Stabilizing subnanometer Ag(0) nanoclusters by thiolate and diphosphine ligands and their crystal structures

NASA Astrophysics Data System (ADS)

Yang, Huayan; Wang, Yu; Zheng, Nanfeng

2013-03-01

The combined use of thiolate and diphosphine as surface ligands helps to stabilize subnanometer Ag(0) nanoclusters, resulting in the successful crystallization of two Ag(0)-containing nanoclusters (Ag16 and Ag32) for X-ray single crystal analysis. Both clusters have core-shell structures with Ag86+ and Ag2212+ as their cores, which are not simply either fragments of face-centered cubic metals or their five-fold twinned counterparts. The clusters display UV-Vis absorption spectra consisting of molecule-like optical transitions.The combined use of thiolate and diphosphine as surface ligands helps to stabilize subnanometer Ag(0) nanoclusters, resulting in the successful crystallization of two Ag(0)-containing nanoclusters (Ag16 and Ag32) for X-ray single crystal analysis. Both clusters have core-shell structures with Ag86+ and Ag2212+ as their cores, which are not simply either fragments of face-centered cubic metals or their five-fold twinned counterparts. The clusters display UV-Vis absorption spectra consisting of molecule-like optical transitions. Electronic supplementary information (ESI) available: Experimental details, more pictures of the structure and XPS spectra of the clusters. CCDC 916463 and 916464. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c3nr34328f

Development of Magnetic Nanomaterials and Devices for Biological Applications

DTIC Science & Technology

2007-10-30

analysis. Suitable crystals for the X-ray diffraction analysis were grown as dark red plates from a saturated hexane solution of [ Co3 (CO)9CCH3] at 4 ºC...Commercially available magnetic nanoparticles are suitable for cell separation where a large number of particles are used to separate a single cell...from a sample. The magnetic moment of these particles is not high enough to enable the separation of single antigen molecules using a single particle

Growth, structural, physical and computational perspectives of trans-4-hydroxy-l-proline: a promising organic nonlinear optical material with large laser-induced damage threshold

NASA Astrophysics Data System (ADS)

Thirumurugan, Ramaiah; Anitha, Kandasamy

2017-05-01

In this work, a systematic study of an organic nonlinear optical (NLO) material, trans-4-hydroxy-l-proline (THP), C5H9NO3 is reported. An optical quality single crystals of THP have been successfully grown by using slow evaporation solution growth technique (SEST). The single crystal x-ray diffraction (SXRD) analysis reveals that grown crystal belongs to the orthorhombic system with non-centrosymmetric space group (NCS), P212121. Powder x-ray diffraction (PXRD) analysis shows relatively a good crystalline nature. The molecular structure of THP was recognized by NMR (1H and 13C) studies and its vibrational modes were confirmed by FTIR and FT-Raman vibrational studies. UV-Vis-NIR spectrum of grown crystal shows high optical transparency in the visible and near-IR region with low near-UV cut-off wavelength at 218 nm. Photoluminescence study confirms ultraviolet wavelength emission of THP crystal. The second harmonic generation (SHG) efficiency of grown crystal is 1.6 times greater with respect to standard potassium dihydrogen phosphate (KDP). Nonlinear refractive index (n 2) and nonlinear absorption coefficient (β) were determined using the Z-scan technique. The title compound owns high thermal stability of 294 °C and specific heat capacity (C P) of 1.21 J g-1 K-1 at 300 K and 11.33 J g-1 K-1 at 539 K (melting point). The laser-induced damage threshold (LDT) value of grown crystal was measured as 7.25 GW cm-2. The crystal growth mechanism and defects of grown crystal were studied by chemical etching technique. Mechanical strength was extensively studied by Vickers microhardness test and crystal void percentage analysis. Moreover, density functional theory (DFT) studies were carried out to probe the Mulliken charge distribution, frontier molecular orbitals (FMOs) and first order hyperpolarizability (β) of the optimized molecular structure to get a better insight of the molecular properties. These characterization results endorse that grown THP crystal as a suitable candidate for NLO applications with large LDT.

Synthesis, crystal growth, structural, thermal and optical properties of naphthalene picrate an organic NLO material.

PubMed

Chandramohan, A; Bharathikannan, R; Kandavelu, V; Chandrasekaran, J; Kandhaswamy, M A

2008-12-01

Crystalline substance of naphthalene picrate (NP) was synthesized and single crystals were grown using slow evaporation solution growth technique. The solubility of the naphthalene picrate complex was estimated using different solvents such as chloroform and benzene. The material was characterized by elemental analysis, powder X-ray diffraction (XRD), nuclear magnetic resonance (NMR) and fourier transform-infrared (FT-IR) techniques. The electronic absorption was studied through UV-vis spectrophotometer. Thermal behavior and stability of the crystal were studied using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The second harmonic generation (SHG) of the material was confirmed using Nd:YAG laser.

Porosity Evolution in a Creeping Single Crystal (Preprint)

DTIC Science & Technology

2012-08-01

1] indicated that the growth of initially present processing induced voids in a nickel based single crystal superalloy played a significant role in...processing induced voids in a nickel based single crystal superalloy played a significant role in limiting creep life. Also, creep tests on single...experimental observations of creep deformation and failure of a nickel based single crystal superalloy, [1, 2]. Metallographic observations have shown that Ni

Study on optical properties of L-valine doped ADP crystal

NASA Astrophysics Data System (ADS)

Shaikh, R. N.; Anis, Mohd.; Shirsat, M. D.; Hussaini, S. S.

2015-02-01

Single crystal of L-valine doped ammonium dihydrogen phosphate has been grown by slow evaporation method at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction technique. The different functional groups of the grown crystal were identified using Fourier transform infrared analysis. The UV-visible studies were employed to examine the high optical transparency and influential optical constants for tailoring materials suitability for optoelectronics applications. The cutoff wavelength of the title crystal was found to be 280 nm with wide optical band gap of 4.7 eV. The dielectric measurements were carried to determine the dielectric constant and dielectric loss at room temperature. The grown crystal has been characterized by thermogravimetric analysis. The second harmonic generation efficiency of the grown crystal was determined by the classical Kurtz powder technique and it is found to be 1.92 times that of potassium dihydrogen phosphate. The grown crystal was identified as third order nonlinear optical material employing Z-scan technique using He-Ne laser operating at 632.8 nm.

Growth and surface topography of WSe{sub 2} single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dixit, Vijay, E-mail: vijdix1@gmail.com; Vyas, Chirag; Pataniya, Pratik

2016-05-06

Tungsten Di-Selenide belongs to the family of TMDCs showing their potential applications in the fields of Optoelectronics and PEC solar cells. Here in the present investigation single crystals of WSe{sub 2} were grown by Direct Vapour Transport Technique in a dual zone furnace having temperature difference of 50 K between the two zones. These single crystals were characterized by EDAX which confirms the stiochiometry of the grown crystals. Surface topography of the crystal was studied by optical micrograph showing the left handed spirals on the surface of WSe{sub 2} crystals. Single crystalline nature of the crystals was confirmed by SAED.

XRD- and infrared-probed anisotropic thermal expansion properties of an organic semiconducting single crystal.

PubMed

Mohanraj, J; Capria, E; Benevoli, L; Perucchi, A; Demitri, N; Fraleoni-Morgera, A

2018-01-17

The anisotropic thermal expansion properties of an organic semiconducting single crystal constituted by 4-hydroxycyanobenzene (4HCB) have been probed by XRD in the range 120-300 K. The anisotropic thermal expansion coefficients for the three crystallographic axes and for the crystal volume have been determined. A careful analysis of the crystal structure revealed that the two different H-bonds stemming from the two independent, differently oriented 4HCB molecules composing the unit cell have different rearrangement patterns upon temperature variations, in terms of both bond length and bond angle. Linearly Polarized Mid InfraRed (LP-MIR) measurements carried out in the same temperature range, focused on the O-H bond spectral region, confirm this finding. The same LP-MIR measurements, on the basis of a semi-empirical relation and of geometrical considerations and assumptions, allowed calculation of the -CNH-O- hydrogen bond length along the a and b axes of the crystal. In turn, the so-calculated -CNH-O- bond lengths were used to derive the thermal expansion coefficients along the corresponding crystal axes, as well as the volumetric one, using just the LP-MIR data. Reasonable to good agreement with the same values obtained from XRD measurements was obtained. This proof-of-principle opens interesting perspectives about the possible development of a rapid, low cost and industry-friendly assessment of the thermal expansion properties of organic semiconducting single crystals (OSSCs) involving hydrogen bonds.

Ultrathin solution-processed single crystals of thiophene-phenylene co-oligomers for organic field-effect devices

NASA Astrophysics Data System (ADS)

Glushkova, Anastasia V.; Poimanova, Elena Yu.; Bruevich, Vladimir V.; Luponosov, Yuriy N.; Ponomarenko, Sergei A.; Paraschuk, Dmitry Yu.

2017-08-01

Thiophene-phenylene co-oligomers (TPCO) single crystals are promising materials for organic light-emitting devices, e.g., light-emitting transistors (OLETs), due to their ability to combine high luminescence and efficient charge transport. However, optical confinement in platy single crystals strongly decreases light emission from their top surface degrading the device performance. To avoid optical waveguiding, single crystals thinner than 100 nm would be beneficial. Herein, we report on solution-processed ultrathin single crystals of TPCO and study their charge transport properties. As materials we used 1,4-bis(5'-hexyl-2,2'-bithiophene-5-yl)benzene (DH-TTPTT) and 1,4-bis(5'-decyl-2,2'-bithiophene-5-yl)benzene (DD-TTPTT). The ultrathin single crystals were studied by optical polarization, atomic-force, and transmission electron microscopies, and as active layers in organic field effect transistors (OFET). The OFET hole mobility was increased tenfold for the oligomer with longer alkyl substituents (DD-TTPTT) reaching 0.2 cm2/Vs. Our studies of crystal growth indicate that if the substrate is wetted, it has no significant effect on the crystal growth. We conclude that solution-processed ultrathin TPCO single crystals are a promising platform for organic optoelectronic field-effect devices.

Nanoparticles Incorporated inside Single-Crystals: Enhanced Fluorescent Properties

DOE PAGES

Liu, Yujing; Zang, Huidong; Wang, Ling; ...

2016-09-25

Incorporation of guest materials inside single-crystalline hosts leads to single-crystal composites that have become more and more frequently seen in both biogenic and synthetic crystals. The unique composite structure together with long-range ordering promises special properties that are, however, less often demonstrated. In this study, we examine the fluorescent properties of quantum dots (QDs) and polymer dots (Pdots) encapsulated inside the hosts of calcite single-crystals. Two CdTe QDs and two Pdots are incorporated into growing calcite crystals, as the QDs and Pdots are dispersed in the crystallization media of agarose gels. As a result, enhanced fluorescent properties are obtained frommore » the QDs and Pdots inside calcite single-crystals with greatly improved photostability and significantly prolonged fluorescence lifetime, compared to those in solutions and gels. Particularly, the fluorescence lifetime increases by 0.5-1.6 times after the QDs or Pdots are incorporated. The enhanced fluorescent properties indicate the advantages of encapsulation by single-crystal hosts that provide dense shells to isolate the fluorescent nanoparticles from atmosphere. As such, this work has implications for advancing the research of single-crystal composites toward their functional design.« less

Giant increase in critical current density of K xFe 2-ySe₂ single crystals

DOE PAGES

Lei, Hechang; Petrovic, C.

2011-12-28

The critical current density Jabc of K xFe 2-ySe₂ single crystals can be enhanced by more than one order of magnitude, up to ~2.1×10⁴ A/cm² by the post annealing and quenching technique. A scaling analysis reveals the universal behavior of the normalized pinning force as a function of the reduced field for all temperatures, indicating the presence of a single vortex pinning mechanism. The main pinning sources are three-dimensional (3D) point-like normal cores. The dominant vortex interaction with pinning centers is via spatial variations in critical temperature T c (“δT c pinning”).

Solar cell structure incorporating a novel single crystal silicon material

DOEpatents

Pankove, Jacques I.; Wu, Chung P.

1983-01-01

A novel hydrogen rich single crystal silicon material having a band gap energy greater than 1.1 eV can be fabricated by forming an amorphous region of graded crystallinity in a body of single crystalline silicon and thereafter contacting the region with atomic hydrogen followed by pulsed laser annealing at a sufficient power and for a sufficient duration to recrystallize the region into single crystal silicon without out-gassing the hydrogen. The new material can be used to fabricate semiconductor devices such as single crystal silicon solar cells with surface window regions having a greater band gap energy than that of single crystal silicon without hydrogen.

Synthesis of mesoporous zeolite single crystals with cheap porogens

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tao Haixiang; Li Changlin; Ren Jiawen

2011-07-15

Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals have been successfully synthesized by adding soluble starch or sodium carboxymethyl cellulose (CMC) to a conventional zeolite synthesis system. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen sorption analysis, {sup 27}Al magic angle spinning nuclear magnetic resonance ({sup 27}Al MAS NMR), temperature-programmed desorption of ammonia (NH{sub 3}-TPD) and ultraviolet-visible spectroscopy (UV-vis). The SEM images clearly show that all zeolite crystals possess the similar morphology with particle size of about 300 nm, the TEM images reveal that irregular intracrystalmore » pores are randomly distributed in the whole crystal. {sup 27}Al MAS NMR spectra indicate that nearly all of the Al atoms are in tetrahedral co-ordination in ZSM-5, UV-vis spectra confirm that nearly all of titanium atoms are incorporated into the framework of TS-1. The catalytic activity of meso-ZSM-5 in acetalization of cyclohexanone and meso-TS-1 in hydroxylation of phenol was also studied. The synthesis method reported in this paper is cost-effective and environmental friendly, can be easily expended to prepare other hierarchical structured zeolites. - Graphical abstract: Mesoporous zeolite single crystals were synthesized by using cheap porogens as template. Highlights: > Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals were synthesized. > Soluble starch or sodium carboxymethyl cellulose (CMC) was used as porogens. > The mesoporous zeolites had connected mesopores although closed pores existed. > Higher catalytic activities were obtained.« less

A Multiscale Computational Model Combining a Single Crystal Plasticity Constitutive Model with the Generalized Method of Cells (GMC) for Metallic Polycrystals.

PubMed

Ghorbani Moghaddam, Masoud; Achuthan, Ajit; Bednarcyk, Brett A; Arnold, Steven M; Pineda, Evan J

2016-05-04

A multiscale computational model is developed for determining the elasto-plastic behavior of polycrystal metals by employing a single crystal plasticity constitutive model that can capture the microstructural scale stress field on a finite element analysis (FEA) framework. The generalized method of cells (GMC) micromechanics model is used for homogenizing the local field quantities. At first, the stand-alone GMC is applied for studying simple material microstructures such as a repeating unit cell (RUC) containing single grain or two grains under uniaxial loading conditions. For verification, the results obtained by the stand-alone GMC are compared to those from an analogous FEA model incorporating the same single crystal plasticity constitutive model. This verification is then extended to samples containing tens to hundreds of grains. The results demonstrate that the GMC homogenization combined with the crystal plasticity constitutive framework is a promising approach for failure analysis of structures as it allows for properly predicting the von Mises stress in the entire RUC, in an average sense, as well as in the local microstructural level, i.e. , each individual grain. Two-three orders of saving in computational cost, at the expense of some accuracy in prediction, especially in the prediction of the components of local tensor field quantities and the quantities near the grain boundaries, was obtained with GMC. Finally, the capability of the developed multiscale model linking FEA and GMC to solve real-life-sized structures is demonstrated by successfully analyzing an engine disc component and determining the microstructural scale details of the field quantities.

A Multiscale Computational Model Combining a Single Crystal Plasticity Constitutive Model with the Generalized Method of Cells (GMC) for Metallic Polycrystals

PubMed Central

Ghorbani Moghaddam, Masoud; Achuthan, Ajit; Bednarcyk, Brett A.; Arnold, Steven M.; Pineda, Evan J.

2016-01-01

A multiscale computational model is developed for determining the elasto-plastic behavior of polycrystal metals by employing a single crystal plasticity constitutive model that can capture the microstructural scale stress field on a finite element analysis (FEA) framework. The generalized method of cells (GMC) micromechanics model is used for homogenizing the local field quantities. At first, the stand-alone GMC is applied for studying simple material microstructures such as a repeating unit cell (RUC) containing single grain or two grains under uniaxial loading conditions. For verification, the results obtained by the stand-alone GMC are compared to those from an analogous FEA model incorporating the same single crystal plasticity constitutive model. This verification is then extended to samples containing tens to hundreds of grains. The results demonstrate that the GMC homogenization combined with the crystal plasticity constitutive framework is a promising approach for failure analysis of structures as it allows for properly predicting the von Mises stress in the entire RUC, in an average sense, as well as in the local microstructural level, i.e., each individual grain. Two–three orders of saving in computational cost, at the expense of some accuracy in prediction, especially in the prediction of the components of local tensor field quantities and the quantities near the grain boundaries, was obtained with GMC. Finally, the capability of the developed multiscale model linking FEA and GMC to solve real-life-sized structures is demonstrated by successfully analyzing an engine disc component and determining the microstructural scale details of the field quantities. PMID:28773458

Microtube-Czochralski technique (μT-CZ):. a novel way of seeding the melt to grow bulk single crystal

NASA Astrophysics Data System (ADS)

Sankaranarayanan, K.; Ramasamy, P.

1998-09-01

A novel microtube seeding has been proposed in the conventional Czochralski pulling technique to grow a bulk single crystal. The versatility of the technique has been shown by adopting this method for the growth of benzil. Benzil single crystals having hexagonal facets are grown by this technique called the microtube-Czochralski technique (μT-CZ). Due to capillary rise, a fine column of melt was crystallized inside the microtube, which leads to the formation of the single crystal nucleation and ends up with hexagonal morphology. The reproducibility for getting single crystal is about 80%. It is evident that this technique is more viable to grow a bulk single crystal from the melt without a pregrown-seed. Further, the proposed μT-CZ technique can also be extended to other newer materials with the proper choice of the microtube.

A novel conformation of gel grown biologically active cadmium nicotinate

NASA Astrophysics Data System (ADS)

Nair, Lekshmi P.; Bijini, B. R.; Divya, R.; Nair, Prabitha B.; Eapen, S. M.; Dileep Kumar, B. S.; Nishanth Kumar, S.; Nair, C. M. K.; Deepa, M.; Rajendra Babu, K.

2017-11-01

The elimination of toxic heavy metals by the formation of stable co-ordination compounds with biologically active ligands is applicable in drug designing. A new crystalline complex of cadmium with nicotinic acid is grown at ambient temperature using the single gel diffusion method in which the crystal structure is different from those already reported. Single crystal x-ray diffraction reveals the identity of crystal structure belonging to monoclinic system, P21/c space group with cell dimensions a = 17.220 (2) Å, b = 10.2480 (2) Å, c = 7.229(9) Å, β = 91.829(4)°. Powder x-ray diffraction analysis confirmed the crystallinity of the sample. The unidentate mode of co-ordination between the metal atom and the carboxylate group is supported by the Fourier Transform Infra Red spectral data. Thermal analysis ensures the thermal stability of the complex. Kinetic and thermodynamic parameters are also calculated. The stoichiometry of the complex is confirmed by the elemental analysis. The UV-visible spectral analysis shows the wide transparency window of the complex in the visible region. The band gap of the complex is found to be 3.92 eV. The complex shows excellent antibacterial and antifungal activity.

Effect of Chain Conformation on the Single-Molecule Melting Force in Polymer Single Crystals: Steered Molecular Dynamics Simulations Study.

PubMed

Feng, Wei; Wang, Zhigang; Zhang, Wenke

2017-02-28

Understanding the relationship between polymer chain conformation as well as the chain composition within the single crystal and the mechanical properties of the corresponding single polymer chain will facilitate the rational design of high performance polymer materials. Here three model systems of polymer single crystals, namely poly(ethylene oxide) (PEO), polyethylene (PE), and nylon-66 (PA66) have been chosen to study the effects of chain conformation, helical (PEO) versus planar zigzag conformation (PE, PA66), and chain composition (PE versus PA66) on the mechanical properties of a single polymer chain. To do that, steered molecular dynamics simulations were performed on those polymer single crystals by pulling individual polymer chains out of the crystals. Our results show that the patterns of force-extension curve as well as the chain moving mode are closely related to the conformation of the polymer chain in the single crystal. In addition, hydrogen bonds can enhance greatly the force required to stretch the polymer chain out of the single crystal. The dynamic breaking and reformation of multivalent hydrogen bonds have been observed for the first time in PA66 at the single molecule level.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, J. R.

We synthesized hexagonal-disc-shaped MgB{sub 2} single crystals under high-pressure conditions and analyzed the microstructure and pinning properties. The lattice constants and the Laue pattern of the crystals from X-ray micro-diffraction showed the crystal symmetry of MgB{sub 2}. A thorough crystallographic mapping within a single crystal showed that the edge and c-axis of hexagonal-disc shape exactly matched the (10-10) and the (0001) directions of the MgB{sub 2} phase. Thus, these well-shaped single crystals may be the best candidates for studying the direction dependences of the physical properties. The magnetization curve and the magnetic hysteresis for these single crystals showed the existencemore » of a wide reversible region and weak pinning properties, which supported our single crystals being very clean.« less

Vertical Bridgman growth and characterization of Cd 0.95-xMn xZn 0.05Te (x=0.20, 0.30) single-crystal ingots

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bolotnikov, A.; Kopach, V.; Kopach, O.

Solid-liquid phase transitions in Cd 0.95-xMn xZn 0.05Te alloys with x = 0.20 and 0.30 were investigated by differential thermal analysis (DTA). The heating/cooling rates were 5 and 10 K/min with a melt dwell time of 10, 30 and 60 minutes. Cd 0.95-xMn xZn 0.05Te (x=0.20, 0.30) single-crystal ingots were grown by the vertical Bridgman method guided using the DTA results. Te inclusions (1-20 microns), typical for CdTe and Cd(Zn)Te crystals, were observed in the ingots by infrared transmission microscopy. The measured X-ray diffraction patterns showed that all compositions are found to be in a single phase. Using current-voltage (I-V)more » measurements, the resistivity of the samples from each ingot was estimated to be about 10 5 Ohm·cm. The optical transmission analysis demonstrated that the band-gap width of the investigated ingots increased from 1.77 to 1.88 eV with the increase of the MnTe content from 20 to 30 mol. %.« less

Comparative study of glycine single crystals with additive of potassium nitrate in different concentration ratios

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gujarati, Vivek P., E-mail: vivekgujarati@gmail.com; Deshpande, M. P., E-mail: vishwadeshpande@yahoo.co.in; Patel, Kamakshi R.

2016-05-06

Semi-organic crystals of Glycine Potassium Nitrate (GPN) with potential applications in Non linear optics (NLO) were grown using slow evaporation technique. Glycine and Potassium Nitrate were taken in three different concentration ratios of 3:1, 2:1 and 1:1 respectively. We checked the solubility of the material in distilled water at different temperatures and could observe the growth of crystals in 7 weeks time. Purity of the grown crystals was confirmed by Energy Dispersive X-ray Analysis (EDAX) and CHN analysis. GSN Powder X-ray diffraction pattern was recorded to confirm the crystalline nature. To confirm the applications of grown crystals in opto-electronics field,more » UV-Vis-NIR study was carried out. Dielectric properties of the samples were studied in between the frequency range 1Hz to 100 KHz.« less

Single-crystal silicon optical fiber by direct laser crystallization

DOE PAGES

Ji, Xiaoyu; Lei, Shiming; Yu, Shih -Ying; ...

2016-12-05

Semiconductor core optical fibers with a silica cladding are of great interest in nonlinear photonics and optoelectronics applications. Laser crystallization has been recently demonstrated for crystallizing amorphous silicon fibers into crystalline form. Here we explore the underlying mechanism by which long single-crystal silicon fibers, which are novel platforms for silicon photonics, can be achieved by this process. Using finite element modeling, we construct a laser processing diagram that reveals a parameter space within which single crystals can be grown. Utilizing this diagram, we illustrate the creation of single-crystal silicon core fibers by laser crystallizing amorphous silicon deposited inside silica capillarymore » fibers by high-pressure chemical vapor deposition. The single-crystal fibers, up to 5.1 mm long, have a very welldefined core/cladding interface and a chemically pure silicon core that leads to very low optical losses down to ~0.47-1dB/cm at the standard telecommunication wavelength (1550 nm). Furthermore, tt also exhibits a photosensitivity that is comparable to bulk silicon. Creating such laser processing diagrams can provide a general framework for developing single-crystal fibers in other materials of technological importance.« less

Resolution of the discrepancy between the variation of the physical properties of Ce 1-xYb xCoIn 5 single crystals and thin films with Yb composition

DOE PAGES

Jang, S.; White, B. D.; Lum, I. K.; ...

2014-11-18

The extraordinary electronic phenomena including an Yb valence transition, a change in Fermi surface topology, and suppression of the heavy fermion quantum critical field at a nominal concentration x≈0.2 have been found in the Ce 1-xYb xCoIn 5 system. These phenomena have no discernable effect on the unconventional superconductivity and normal-state non-Fermi liquid behaviour that occur over a broad range of x up to ~0.8. However, the variation of the coherence temperature T* and the superconducting critical temperature T c with nominal Yb concentration x for bulk single crystals is much weaker than that of thin films. To determine whethermore » differences in the actual Yb concentration of bulk single crystals and thin film samples might be responsible for these discrepancies, we employed Vegard’s law and the spectroscopically determined values of the valences of Ce and Yb as a function of x to determine the actual composition x act of bulk single crystals. This analysis is supported by energy-dispersive X-ray spectroscopy, wavelength-dispersive X-ray spectroscopy, and transmission X-ray absorption edge spectroscopy measurements. The actual composition x act is found to be about one-third of the nominal concentration x up to x~0.5, and resolves the discrepancy between the variation of the physical properties of Ce 1-xYb xCoIn 5 single crystals and thin films with Yb concentration.« less

Formation of curved micrometer-sized single crystals.

PubMed

Koifman Khristosov, Maria; Kabalah-Amitai, Lee; Burghammer, Manfred; Katsman, Alex; Pokroy, Boaz

2014-05-27

Crystals in nature often demonstrate curved morphologies rather than classical faceted surfaces. Inspired by biogenic curved single crystals, we demonstrate that gold single crystals exhibiting curved surfaces can be grown with no need of any fabrication steps. These single crystals grow from the confined volume of a droplet of a eutectic composition melt that forms via the dewetting of nanometric thin films. We can control their curvature by controlling the environment in which the process is carried out, including several parameters, such as the contact angle and the curvature of the drops, by changing the surface tension of the liquid drop during crystal growth. Here we present an energetic model that explains this phenomenon and predicts why and under what conditions crystals will be forced to grow with the curvature of the microdroplet even though the energetic state of a curved single crystal is very high.

Spectroscopic analysis and efficient diode-pumped 1.9 μm Tm3+-doped β'-Gd2(MoO4)3 crystal laser.

PubMed

Tang, Jianfeng; Chen, Yujin; Lin, Yanfu; Gong, Xinghong; Huang, Jianhua; Luo, Zundu; Huang, Yidong

2011-07-04

Tm3+-doped β'-Gd2(MoO4)3 single crystal was grown by the Czochralski method. Spectroscopic analysis was carried out along different polarizations. End-pumped by a quasi-cw diode laser at 795 nm in a plano-concave cavity, an average laser output power of 58 mW around 1.9 μm was achieved in a 0.93-mm-thick crystal when the output coupler transmission was 7.1%. The absorbed pump threshold was 8 mW and the slope efficiency of the laser was 57%. This crystal has smooth and broad gain curve around 1.9 μm, which shows that it is also a potential gain medium for tunable and short pulse lasers.

Capillarity creates single-crystal calcite nanowires from amorphous calcium carbonate.

PubMed

Kim, Yi-Yeoun; Hetherington, Nicola B J; Noel, Elizabeth H; Kröger, Roland; Charnock, John M; Christenson, Hugo K; Meldrum, Fiona C

2011-12-23

Single-crystal calcite nanowires are formed by crystallization of morphologically equivalent amorphous calcium carbonate (ACC) particles within the pores of track etch membranes. The polyaspartic acid stabilized ACC is drawn into the membrane pores by capillary action, and the single-crystal nature of the nanowires is attributed to the limited contact of the intramembrane ACC particle with the bulk solution. The reaction environment then supports transformation to a single-crystal product. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Laser radiation frequency doubling in a single-crystal fibre based on a stoichiometric LiNbO3 crystal

NASA Astrophysics Data System (ADS)

Kashin, V. V.; Nikolaev, D. A.; Rusanov, S. Ya; Tsvetkov, V. B.

2015-01-01

We demonstrate the employment of single-crystal optical fibres based on lithium niobate for doubling the laser radiation frequency. The measured characteristics of the fibre confirm its high quality and spatial homogeneity. Parameters of the frequency doublers for neodymium laser radiation (λ = 1 mm) based on fibre and bulk single crystals are compared. Single crystals are grown by the method of laser-heated pedestal growing with heating by radiation of a CO2 laser (LHPG-method).

Identification and Control of Gravity Related Defect Formation During Melt Growth of Electro-Optic Single Crystals Bismuth Silicate(Bi12SiO20)

NASA Technical Reports Server (NTRS)

Becia, Piotr; Wiegel, Michaela E. K.

2004-01-01

A research carried out under Award Number NAG8-1487 was aimed at to the design, conduct and analysis of experiments directed at the identification and control of gravitational effects on crystal growth, segregation and defect formation in the Sillenite system: bismuth silicate (Bi(12)SiO(20)). Correlation analyses was conducted in order to establish the influence of gravity related defects introduced during crystal growth on critical, application specific properties. Achievement of the states objective was conducted during the period from Feb. 01, 1998 to Dec. 31, 2003 with the following anticipated milestones: 1. Establishment of capabilities for (a) reproducible Czochralski and Bridgman-type growth of BSO single crystals and (b) for comprehensive analysis of crystalline and chemical defects as well as for selective property characterization of grown crystals (year 1). 2. Design and execution of critical space growth experiment(s) based on analyses of prefatory space results (experiments aimed at establishing the viability of planned approaches and procedures) and on unresolved issues related to growth, segregation and defect formation associated with conventional growth in Bridgman geometries. Comparative analysis of growth under conventional and under mu-g conditions; identification of gravity related defect formation during conventional Bridgman growth and formulation of approaches for their control (years 2 and 3). Development of charge confinement system which permits growth interface demarcation (in a mu-g environment) as well as minimization of confinement related stress and contamination during growth; design of complementary mu-g growth experiments aimed at quantitative mu-g growth and segregation analyses (year 4). 3. Conduct of quantitative mu-g growth experiments directed at: (a) identification and control of gravity related crystalline and chemical defect formation during single crystal growth of Bi(12)SiO(20) and at (b) defect engineering -the development of approaches to the controlled generation during crystal growth of specified point defects in homogeneous distribution (year 5). The proposed research places focus on a class of materials which have outstanding electrical and optical properties but have so far failed to reach their potential, primarily because of our inability to control adequately their stoichiometry and crystal defect formation as well as confinement related contamination and lattice stress.

Positioning and joining of organic single-crystalline wires

PubMed Central

Wu, Yuchen; Feng, Jiangang; Jiang, Xiangyu; Zhang, Zhen; Wang, Xuedong; Su, Bin; Jiang, Lei

2015-01-01

Organic single-crystal, one-dimensional materials can effectively carry charges and/or excitons due to their highly ordered molecule packing, minimized defects and eliminated grain boundaries. Controlling the alignment/position of organic single-crystal one-dimensional architectures would allow on-demand photon/electron transport, which is a prerequisite in waveguides and other optoelectronic applications. Here we report a guided physical vapour transport technique to control the growth, alignment and positioning of organic single-crystal wires with the guidance of pillar-structured substrates. Submicrometre-wide, hundreds of micrometres long, highly aligned, organic single-crystal wire arrays are generated. Furthermore, these organic single-crystal wires can be joined within controlled angles by varying the pillar geometries. Owing to the controllable growth of organic single-crystal one-dimensional architectures, we can present proof-of-principle demonstrations utilizing joined wires to allow optical waveguide through small radii of curvature (internal angles of ~90–120°). Our methodology may open a route to control the growth of organic single-crystal one-dimensional materials with potential applications in optoelectronics. PMID:25814032

Controlling the surface termination of NdGaO3 (110): the role of the gas atmosphere.

PubMed

Cavallaro, Andrea; Harrington, George F; Skinner, Stephen J; Kilner, John A

2014-07-07

In this work the effect of gas atmosphere on the surface termination reconstruction of single crystal NdGaO3 (110) (NGO) during thermal annealing was analyzed. Using Low Energy Ion Scattering (LEIS) it has been possible to study the chemical composition of the first atomic layer of treated NGO single crystal samples. NGO has been analyzed both as-received and after a specific thermal treatment at 1000 °C under different gas fluxes (argon, nitrogen, static air, synthetic air, nitrogen plus 5% hydrogen and wet synthetic air respectively). Thermal annealing of perovskite single crystals, as already reported in the literature, is used to obtain a fully A-cation surface termination. Nevertheless the effect of the gas-atmosphere on this process has not been previously reported. By the use of sequential low energy Ar(+) sputtering combined with the primary ion LEIS analysis, the reconstruction of the outermost atomic layers has allowed the clarification of the mechanism of NGO neodymium surface enrichment. It is proposed that the gallium at the surface is submitted to a reduction/evaporation mechanism caused by low oxygen partial pressure and/or high water pressure in the vector gas. Below the first surface atomic layers of an as-received NGO single-crystal a gallium-rich phase has also been observed.

Solid-state reaction kinetics and optical studies of cadmium doped magnesium hydrogen phosphate crystals

NASA Astrophysics Data System (ADS)

Verma, Madhu; Gupta, Rashmi; Singh, Harjinder; Bamzai, K. K.

2018-04-01

The growth of cadmium doped magnesium hydrogen phosphate was successfully carried out by using room temperature solution technique i.e., gel encapsulation technique. Grown crystals were confirmed by single crystal X-ray diffraction (XRD). The structure of the grown crystal belongs to orthorhombic crystal system and crystallizes in centrosymmetric space group. Kinetics of the decomposition of the grown crystals were studied by non-isothermal analysis. Thermo gravimetric / differential thermo analytical (TG/DTA) studies revealed that the grown crystal is stable upto 119 °C. The various steps involved in the thermal decomposition of the material have been analysed using Horowitz-Metzger, Coats-Redfern and Piloyan-Novikova equations for evaluating various kinetic parameters. The optical studies shows that the grown crystals possess wide transmittance in the visible region and significant optical band gap of 5.5ev with cut off wavelength of 260 nm.

Eye-Safe Polycrystalline Lasers

DTIC Science & Technology

2013-03-01

developed novel ceramic and single crystal laser gain media as a platform for power scaling to +100 kW class levels. Hydrothermal techniques were used...order of magnitude improvement in purity. Bulk single crystal growth was demonstrated for scandia and lutetia single crystals , as well as several...exhibited equivalent transparency to that of the single crystal in the near-infrared spectral region and initial lasing results have been successful

Single crystalline hollow metal-organic frameworks: a metal-organic polyhedron single crystal as a sacrificial template.

PubMed

Kim, Hyehyun; Oh, Minhak; Kim, Dongwook; Park, Jeongin; Seong, Junmo; Kwak, Sang Kyu; Lah, Myoung Soo

2015-02-28

Single crystalline hollow metal-organic frameworks (MOFs) with cavity dimensions on the order of several micrometers and hundreds of micrometers were prepared using a metal-organic polyhedron single crystal as a sacrificial hard template. The hollow nature of the MOF crystal was confirmed by scanning electron microscopy of the crystal sliced using a focused ion beam.

The first 3-D LaIII-SrII heterometallic complex: Synthesis, structure and luminescent properties

NASA Astrophysics Data System (ADS)

Hong, Zhiwei; Ran, Jingwen; Li, Tao; Chen, Yanmei

2016-10-01

The first 3-D LaIII-SrII heterometallic complex, namely [La2Sr(pda)4(H2O)4]n·6nH2O (1, H2pda = pyridine-2,6-dicarboxylic acid), has been successfully synthesized under solvothermal conditions. Single crystal X-ray diffraction analysis reveals that complex 1 features a 3-D porous framework and displays a new topology. The crystal structure can be simplified to a 4,6-connected 3-D network with Schläfli symbol of {34·42·88·9}2{34·42}. The crystals also have been characterized by X-ray powder diffraction, elemental analysis, thermal analysis, and IR spectroscopy. The infrared spectral analysis indicates that complex 1 is a carboxylate coordinated compound, several water molecules exist in the compound. The thermal study shows that there are ten water molecules in the crystal structure. The luminescent property has also been investigated. It shows a blue-purple fluorescence emission.

The solid state of rebamipide: preparation, characterization, and dissolution.

PubMed

Jeon, Seong Hyeon; Sohn, Young Taek

2016-04-01

Rebamipide is marketed as a peptic ulcer agent under the trade name Mucosta(R). The objective of this work was to investigate the existence of polymorphs and pseudopolymorphs of rebamipide. Two crystal forms of rebamipide were isolated by recrystallization and characterized by differential thermal analysis (DTA), thermogravimetric analysis (TG), powder X-ray diffractometry, infrared spectrometry, and nuclear magnetic resonance. The DTA curve of Form 1 showed one endothermic peak at 305.2 °C, and that of Form 2 showed one endothermic peak at 307.3 °C. The TG curve of Form 1 showed a single weight loss at 305.2 °C, which corresponded to melting. The TG curve of Form 2 also showed a single weight loss at 307.3 °C, which corresponded to melting. The melting point of Form 2 was higher than that of Form 1. In the dissolution studies in pH 6.8 buffer at 37 ± 0.5 °C, the two crystal forms showed no significant differences in dissolution. After 3 months of storage at 0, 52, and 95% RH, the two crystal forms were not transformed. After milling with a Specamill for 2 h, the two crystal forms were not transformed.

Wafer-scale single-crystal perovskite patterned thin films based on geometrically-confined lateral crystal growth

PubMed Central

Lee, Lynn; Baek, Jangmi; Park, Kyung Sun; Lee, Yong-EunKoo; Shrestha, Nabeen K.; Sung, Myung M.

2017-01-01

We report a facile roll-printing method, geometrically confined lateral crystal growth, for the fabrication of large-scale, single-crystal CH3NH3PbI3 perovskite thin films. Geometrically confined lateral crystal growth is based on transfer of a perovskite ink solution via a patterned rolling mould to a heated substrate, where the solution crystallizes instantly with the immediate evaporation of the solvent. The striking feature of this method is that the instant crystallization of the feeding solution under geometrical confinement leads to the unidirectional lateral growth of single-crystal perovskites. Here, we fabricated single-crystal perovskites in the form of a patterned thin film (3 × 3 inch) with a high carrier mobility of 45.64 cm2 V−1 s−1. We also used these single-crystal perovskite thin films to construct solar cells with a lateral configuration. Their active-area power conversion efficiency shows a highest value of 4.83%, which exceeds the literature efficiency values of lateral perovskite solar cells. PMID:28691697

Mosaic anisotropy model for magnetic interactions in mesostructured crystals

NASA Astrophysics Data System (ADS)

Goldman, Abby R.; Asenath-Smith, Emily; Estroff, Lara A.

2017-10-01

We propose a new model for interpreting the magnetic interactions in crystals with mosaic texture called the mosaic anisotropy (MA) model. We test the MA model using hematite as a model system, comparing mosaic crystals to polycrystals, single crystal nanoparticles, and bulk single crystals. Vibrating sample magnetometry confirms the hypothesis of the MA model that mosaic crystals have larger remanence (Mr/Ms) and coercivity (Hc) compared to polycrystalline or bulk single crystals. By exploring the magnetic properties of mesostructured crystalline materials, we may be able to develop new routes to engineering harder magnets.

Growth Temperature Dependence of Morphology of GaN Single Crystals in the Na-Li-Ca Flux Method

NASA Astrophysics Data System (ADS)

Wu, Xi; Hao, Hangfei; Li, Zhenrong; Fan, Shiji; Xu, Zhuo

2018-02-01

In this paper, the effect of growth temperature on the morphology and transparency of the GaN crystals obtained by the Li-Ca-added Na Flux method was studied. Addition of Li-Ca was attempted to control the growth habit and further improve transparency of GaN crystals. The samples with wurtzite structure of GaN were confirmed by the x-ray powder diffraction analysis. GaN single crystal with maximum size of about 6 mm was grown at 750°C. As the growth temperature was increased from 700°C to 850°C, the morphology of the crystals changed from pyramid to prism, and their surfaces became smooth. It was found that high growth temperature was beneficial to obtain a transparent crystal, but the evaporation of sodium would suppress its further growth. The E 2 (high) mode in the Raman spectra was at 568 cm-1, and the full-width at half-maximum values of this peak for the crystals obtained at 700°C, 750°C, 800°C, and 850°C were 7.5 cm-1, 10.3 cm-1, 4.4 cm-1, and 4.0 cm-1, respectively. It indicates that all the crystals are stress free and the transparent crystal grown at high temperature has high structural quality or low impurity concentrations.

Supramolecular network through Nsbnd H…O, Osbnd H…O and Csbnd H…O hydrogen bonding interaction and density functional theory studies of 4-methylanilinium-3-carboxy-4-hydroxybenzenesulphonate crystal

NASA Astrophysics Data System (ADS)

Rajkumar, M.; Muthuraja, P.; Dhandapani, M.; Chandramohan, A.

2018-02-01

By utilizing the hydrogen bonding strategy, 4-methylanilinium-3-hydroxy-4-corboxy-benzenesulphonate (4MABS), an organic proton transfer molecular salt was synthesized and single crystals of it were successfully grown by slow solvent evaporation solution growth technique at ambient temperature. The 1H and 13C NMR spectra were recorded to establish the molecular structure of the title salt. The single crystal XRD analysis reveals that the title salt crystallizes in monoclinic crystal system with centrosymmetric space group, P21/n. Further, the title salt involves extensive intermolecular Nsbnd H…O, Osbnd H…O and Csbnd H…O as well as intramolecular Osbnd H…O hydrogen bonding interactions to construct supramolecular architecture. All quantum chemical calculations were performed at the level of density functional theory (DFT) with B3LYP functional using 6-311G (d,p) basis atomic set. The photoluminescence spectrum was recorded to explore the emission property of the title crystal. The presence of the various vibrational modes and functional groups in the synthesized salt was confirmed by FT-IR studies. The thermal behaviour of title crystal was established employing TG/DTA analyses. The mechanical properties of the grown crystal were determined by Vicker's microhardness studies. Dielectric measurements were carried out on the grown crystal at a different temperature to evaluate electrical properties.

Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

NASA Astrophysics Data System (ADS)

Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

2012-04-01

A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

Crystal growth and magneto-transport behavior of PdS1-δ

NASA Astrophysics Data System (ADS)

Cao, Lin; Lv, Yang-Yang; Chen, Si-Si; Li, Xiao; Zhou, Jian; Yao, Shu-Hua; Chen, Y. B.; Lu, Minghui; Chen, Yan-Feng

2018-04-01

PdS is theoretically proposed to novel topological material with eight-band fermions. Here, PdS1-δ crystals were successfully grown from KI as solvent by modified flux method. The single crystalline quality and compositional homogeneity of grown PdS1-δ are characterized by X-ray diffraction and energy dispersion spectroscopy. Temperature dependent electrical transport property of PdS1-δ demonstrates a semiconductor-like behavior. Analysis of temperature-dependent resistance indicates that there is variable-range-hopping behavior at low temperature. The clear negative MR of PdS1-δ single crystals is measured at the low temperature (<30 K), which may be ascribed to the interaction between conducting carriers and localized moments. however, the magneto-transport results have not shown the clues of topological feature of PdS.

Synthesis, spectral, thermal, X-ray single crystal of new RuCl₂(dppb)diamine complexes and their application in hydrogenation of Cinnamic aldehyde.

PubMed

Warad, Ismail; Al-Hussain, Hanan; Al-Far, Rawhi; Mahfouz, Refaat; Hammouti, Belkheir; Hadda, Taibi Ben

2012-09-01

The preparation of new three trans-[RuCl(2)(dppb)(N-N)] with mixed diamine (N-N) and 1,4-bis-(diphenylphosphino)butane (dppb) ligands, starting from RuCl(2)(PPh(3))(3) as precursor is presented. The complexes are characterized on the basis of elemental analysis, IR, (1)H, (13)C and (31)P{(1)H}NMR, FAB-MS, TG/DTA and single crystal X-ray diffraction studies. Complex (2L(1)) crystallizes in the monoclinic unit cells with the space group P2(1). The catalysts are evaluated for their Cinnamic aldehyde hydrogenation. The catalysts show excellent activity and selectivity for the unsaturated carbonyl compound under mild conditions. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, crystal structures and luminescence properties of new multi-component co-crystals of isostructural Co(II) and Zn(II) complexes

NASA Astrophysics Data System (ADS)

Tella, Adedibu C.; Owalude, Samson O.; Omotoso, Mary F.; Olatunji, Sunday J.; Ogunlaja, Adeniyi S.; Alimi, Lukman O.; Popoola, Olugbenga K.; Bourne, Susan A.

2018-04-01

Two novel isostructural compounds containing multi-component co-crystals [M(C6H4NO2)2(H2O)2](C9H6O6)2 (M = Co (1), Zn (2), C6H4NO2 = Picolinic acid, C9H6O6 = Trimesic acid) have been synthesized. The compounds were characterized by elemental analysis, FT-IR, UV-Visible and 1H NMR spectroscopies as well as thermal and single crystal X-ray diffraction analyses. Single crystal X-ray diffraction analysis reveals that 1 and 2 are isostructural. Compound 1 crystallizes in triclinic space group (P-1, with a = 5.154 (10) Å, b = 11.125 (2) Å, c = 14.113 (3) Å, α = 91.01 (3)°, β = 100.54 (3)°, and γ = 102.71 (3)°). In a similar fashion, compound 2 crystallizes in triclinic space group (P-1, with a = 5.1735 (3) Å, b = 11.0930 (10) Å, c = 14.1554 (8) Å, α = 91.70 (3)°, β = 100.26 (3)°, γ = 102.90 (3)°). The metal (II) cation presents distorted MN2O4 octahedral geometry with H2O molecules coordinated to the metal in equatorial position while the picolinic acid molecules are axially coordinated through the pyridine N atom. The two trimesic acid molecules are not part of the first coordination sphere. Compounds 1 and 2 constitute an example of a class of coordination compound of multicomponent crystals having trimesic acid outside the coordination sphere where it is neither protonated or deprotonated. The two compounds were investigated for luminiscence properties.

Patterned solid state growth of barium titanate crystals

NASA Astrophysics Data System (ADS)

Ugorek, Michael Stephen

An understanding of microstructure evolution in ceramic materials, including single crystal development and abnormal/enhanced grain growth should enable more controlled final ceramic element structures. In this study, two different approaches were used to control single crystal development in a patterned array. These two methods are: (1) patterned solid state growth in BaTiO 3 ceramics, and (2) metal-mediated single crystal growth in BaTiO 3. With the patterned solid state growth technique, optical photolithography was used to pattern dopants as well as [001] and [110] BaTiO3 single crystal template arrays with a 1000 microm line pattern array with 1000 microm spacings. These patterns were subsequently used to control the matrix grain growth evolution and single crystal development in BaTiO3. It was shown that the growth kinetics can be controlled by a small initial grain size, atmosphere conditions, and the introduction of a dopant at selective areas/interfaces. By using a PO2 of 1x10-5 atm during high temperature heat treatment, the matrix coarsening has been limited (to roughly 2 times the initial grain size), while retaining single crystal boundary motion up to 0.5 mm during growth for dwell times up to 9 h at 1300°C. The longitudinal and lateral growth rates were optimized at 10--15 microm/h at 1300°C in a PO2 of 1x10 -5 atm for single crystal growth with limited matrix coarsening. Using these conditions, a patterned microstructure in BaTiO3 was obtained. With the metal-mediated single crystal growth technique, a novel approach for fabricating 2-2 single crystal/polymer composites with a kerf < 5 microns was demonstrated. Surface templated grain growth was used to propagate a single crystal interface into a polycrystalline BaTiO3 or Ba(Zr0.05 Ti0.95)O3 matrix with lamellar nickel layers. The grain growth evolution and texture development were studied using both [001] and [110] BaTiO3 single crystals templates. By using a PO 2 of 1x10-11 atm during high temperature heat treatment, matrix coarsening was limited while enabling single crystal boundary motion up to 0.35 mm during growth between 1250°C and 1300°C with growth rates ˜ 3--4 microm/h for both single crystal orientations. By removing the inner electrodes, 2-2 single crystal (or ceramic) composites were prepared. The piezoelectric and dielectric properties of the composites of the two compositions were measured. The d33 and d31 of the composites were similar to the polycrystalline ceramic of the same composition.

The evolution of machining-induced surface of single-crystal FCC copper via nanoindentation

NASA Astrophysics Data System (ADS)

Zhang, Lin; Huang, Hu; Zhao, Hongwei; Ma, Zhichao; Yang, Yihan; Hu, Xiaoli

2013-05-01

The physical properties of the machining-induced new surface depend on the performance of the initial defect surface and deformed layer in the subsurface of the bulk material. In this paper, three-dimensional molecular dynamics simulations of nanoindentation are preformed on the single-point diamond turning surface of single-crystal copper comparing with that of pristine single-crystal face-centered cubic copper. The simulation results indicate that the nucleation of dislocations in the nanoindentation test on the machining-induced surface and pristine single-crystal copper is different. The dislocation embryos are gradually developed from the sites of homogeneous random nucleation around the indenter in the pristine single-crystal specimen, while the dislocation embryos derived from the vacancy-related defects are distributed in the damage layer of the subsurface beneath the machining-induced surface. The results show that the hardness of the machining-induced surface is softer than that of pristine single-crystal copper. Then, the nanocutting simulations are performed along different crystal orientations on the same crystal surface. It is shown that the crystal orientation directly influences the dislocation formation and distribution of the machining-induced surface. The crystal orientation of nanocutting is further verified to affect both residual defect generations and their propagation directions which are important in assessing the change of mechanical properties, such as hardness and Young's modulus, after nanocutting process.

Electron paramagnetic resonance study of radiation-induced paramagnetic centers in succinic anhydride single crystal

NASA Astrophysics Data System (ADS)

Caliskan, Betul; Caliskan, Ali Cengiz; Er, Emine

2017-09-01

Succinic anhydride single crystals were exposed to 60Co-gamma irradiation at room temperature. The irradiated single crystals were investigated at 125 K by Electron Paramagnetic Resonance (EPR) Spectroscopy. The investigation of EPR spectra of irradiated single crystals of succinic anhydride showed the presence of two succinic anhydride anion radicals. The anion radicals observed in gamma-irradiated succinic anhydride single crystal were created by the scission of the carbon-oxygen double bond. The structure of EPR spectra demonstrated that the hyperfine splittings arise from the same radical species. The reduction of succinic anhydride was identified which is formed by the addition of an electron to oxygen of the Csbnd O bond. The g values, the hyperfine structure constants and direction cosines of the radiation damage centers observed in succinic anhydride single crystal were obtained.

Growth and characterization of Yb:Ho:YAG single crystal fiber

NASA Astrophysics Data System (ADS)

Yang, Yilun; Ye, Linhua; Bao, Renjie; Li, Shanming; Zhang, Peixiong; Xu, Min; Hang, Yin

2018-06-01

High quality Yb and Ho co-doped Y3Al5O12 single crystal fibers have been successfully grown by the laser heated pedestal growth method of up to 124 mm in length and 450 μm in diameter for the first time. The results of inductively coupled plasma-atomic emission spectrometry analysis, X-ray diffraction and Raman spectroscopy reveal that the lattice structure and doping concentrations of the SCF are the same as that of the bulk. Scanning electron microscopy microphotographs shows that the fibers only have minor diameter fluctuations within 0.5%.

Spherical nanoindentation stress-strain curves of commercially pure titanium and Ti-6Al-4V

DOE Data Explorer

Weaver, Jordan S. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Priddy, Matthew W. [Georgia Inst. of Technology, Atlanta, GA (United States); McDowell, David L. [Georgia Inst. of Technology, Atlanta, GA (United States); Kalidindi, Surya R. [Georgia Inst. of Technology, Atlanta, GA (United States)

2016-07-27

Spherical nanoindentation combined with electron back-scattered diffraction was employed to characterize the grain-scale elastic and plastic anisotropy of single crystal alpha-Ti for commercially pure (CP-Ti) and alloyed (Ti-64) titanium. In addition, alpha-beta Ti (single colony) grains were characterized. The data set includes the nanoindentation force, displacement, and contact stiffness, the nanoindentation stress-strain analysis, and the alpha-Ti crystal orientations. Details of the samples and experimental protocols can be found in Weaver et al. (2016) Acta Materialia doi:10.1016/j.actamat.2016.06.053.

The influence of severe plastic deformation by high pressure torsion on structure and mechanical properties of Hadfield steel single crystals

NASA Astrophysics Data System (ADS)

Zakharova, G. G.; Astafurova, E. G.

2010-07-01

Hadfield steel single crystals have been deformed by high pressure torsion at room temperature (P=5GPa) for 1, 2, 3 revolutions. The resulting microstructure has been studied by means of transmission electron microscopy (TEM) and X-ray analysis. The size of fragments decreases with increasing number of revolutions due to interaction of slip dislocations, microbands and thin twins. As a result of severe plastic deformation, the microhardness of the Hadfield steel has been increased, and a portion of epsilon, α' martensite has been found.

Hydrogen positions in single nanocrystals revealed by electron diffraction

NASA Astrophysics Data System (ADS)

Palatinus, L.; Brázda, P.; Boullay, P.; Perez, O.; Klementová, M.; Petit, S.; Eigner, V.; Zaarour, M.; Mintova, S.

2017-01-01

The localization of hydrogen atoms is an essential part of crystal structure analysis, but it is difficult because of their small scattering power. We report the direct localization of hydrogen atoms in nanocrystalline materials, achieved using the recently developed approach of dynamical refinement of precession electron diffraction tomography data. We used this method to locate hydrogen atoms in both an organic (paracetamol) and an inorganic (framework cobalt aluminophosphate) material. The results demonstrate that the technique can reliably reveal fine structural details, including the positions of hydrogen atoms in single crystals with micro- to nanosized dimensions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

Single crystals of selected titanates and tungstates

NASA Technical Reports Server (NTRS)

Loiacono, G. M.

1972-01-01

The compound preparation and crystal growth of a number of mixed titanate compositions was investigated. None of the compounds studied were found to melt congruently and therefore, crystal growth was extremely difficult. Various single crystal preparation methods always resulted in mixed phases from which 1-2 mm size crystals could be separated. It is concluded from this study that before successful single crystal growth can be accomplished, a detailed study of the phase diagrams in each of the systems of interest must be completed.

Interface Character of Aluminum-Graphite Metal Matrix Composites.

DTIC Science & Technology

1983-01-27

studied included the commer- cial A/graphite composites; layered model systems on single crystal and poly- crystalline graphite substrates as well as...composition and thickness of the composite interface, and graphite crystal orientation. 3 For the model systems in this study , single crystal graphite...been reviewed by Kingcry. Segregation at surfaces in single- crystal MgO of Fe, Cr and Sc, which were Dresent in concentrations within the single- 3phase

Magnetic spherical cores partly coated with periodic mesoporous organosilica single crystals.

PubMed

Li, Jing; Wei, Yong; Li, Wei; Deng, Yonghui; Zhao, Dongyuan

2012-03-07

Core-shell structured materials are of special significance in various applications. Until now, most reported core-shell structures have polycrystalline or amorphous coatings as their shell layers, with popular morphologies of microspheres or quasi-spheres. However, the single crystals, either mesoscale or atomic ones, are still rarely reported as shell layers. If single crystals can be coated on core materials, it would result in a range of new type core-shell structures with various morphologies, and probably more potential applications. In this work, we demonstrate that periodic mesoporous organosilica (PMO) single crystals can partly grow on magnetic microspheres to form incomplete Fe(3)O(4)@nSiO(2)@PMO core-shell materials in aqueous solution, which indeed is the first illustration that mesoporous single-crystal materials can be used as shell layers for preparation of core-shell materials. The achieved materials have advantages of high specific surface areas, good magnetic responses, embedded functional groups and cubic mesopore channels, which might provide them with various application conveniences. We suppose the partial growth is largely decided by the competition between growing tendency of single crystals and the resistances to this tendency. In principle, other single crystals, including a range of atomic single crystals, such as zeolites, are able to be developed into such core-shell structures.

Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

NASA Astrophysics Data System (ADS)

Wang, W. H.; Ren, X.

2006-04-01

We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

Bulk growth of undoped and Nd3+ doped zinc thiourea chloride (ZTC) monocrystal: Exploring the remarkably enhanced structural, optical, electrical and mechanical performance of Nd3+ doped ZTC crystal for NLO device applications

NASA Astrophysics Data System (ADS)

Anis, Mohd; Muley, Gajanan. G.

2017-05-01

In current scenario good quality crystals are demanded for NLO device application hence present communication is aimed to grow bulk crystal and investigate the doping effect of rare earth element Nd3+ on structural, linear-nonlinear optical, luminescence, mechanical and dielectric properties of zinc thiourea chloride (ZTC) crystal. The ZTC crystal of dimension 21×10×8 mm3 and the Nd3+ doped ZTC crystal of dimension 27×17×5 mm3 have been grown from aqueous solution by slow evaporation technique. The elemental analysis of Nd3+ doped ZTC single crystal has been performed by means of energy dispersive spectroscopic technique. The powder X-ray diffraction technique has been employed to confirm the crystalline phase and identify the effect of Nd3+ doping on structural dimensions of ZTC crystal. The grown crystals have been characterized by UV-Vis-NIR study in the range of 190-1100 nm to ascertain the enhancement in optical transparency of ZTC crystal facilitated by dopant Nd3+. The recorded transmittance data has been utilized to investigate the vital optical constants of grown crystals. The second order nonlinear optical behavior of grown crystals has been evaluated by means of Kurtz-Perry test and the second harmonic generation efficiency of Nd3+ doped ZTC crystal is found to be 1.24 times higher than ZTC crystal. The luminescence analysis has been performed to examine the electronic purity and the color centered photoluminescence emission nature of pure and Nd3+ doped ZTC crystals. The influence of Nd3+ ion on mechanical behavior of ZTC crystal has been investigated by means of microhardness studies. The nature of dielectric constant and dielectric loss of pure and Nd3+ doped ZTC crystal has been examined in the range of 40-100 °C under dielectric study. The Z-scan technique has been employed using the He-Ne laser to investigate the third order nonlinear optical (TONLO) nature of Nd3+ doped ZTC single crystal. The magnitude of TONLO susceptibility, absorption coefficient and refraction has been determined using the Z-scan transmittance data.

EPR study of free radical in gamma-irradiated bis(cyclopentadienyl)zirconium dichloride single crystal

NASA Astrophysics Data System (ADS)

Caliskan, Betul; Caliskan, Ali Cengiz

2017-06-01

Bis(cyclopentadienyl)zirconium dichloride (BCZD; zirconocene dichloride) single crystals were exposed to 60Co-γ irradiation at room temperature. The irradiated single crystals were investigated between 125 and 470 K by electron paramagnetic resonance spectroscopy. The spectra of the crystals were found to be temperature independent. The paramagnetic center was attributed to the cyclopentadienyl radical. The g values of the radiation damage center observed in BCZD single crystal and the hyperfine structure constants of the free electron with nearby protons were obtained.

Orientation and temperature dependence of some mechanical properties of the single-crystal nickel-base superalloy Rene N4. 3: Tension-compression anisotropy

NASA Technical Reports Server (NTRS)

Miner, R. V.; Gaab, T. P.; Gayda, J.; Hemker, K. J.

1985-01-01

Single crystal superalloy specimens with various crystallographic directions along their axes were tested in compression at room temperature, 650, 760, 870, and 980 deg C. These results are compared with the tensile behavior studied previously. The alloy, Rene N4, was developed for gas turbine engine blades and has the nominal composition 3.7 Al, 4.2 Ti, 4 Ta, 0.5 Nb, 6 W, 1.5 Mo 9 Cr. 7.5 Co, balance Ni, in weight percent. Slip trace analysis showed that primary cube slip occurred even at room temperature for the 111 specimens. With increasing test temperature more orientations exhibited primary cube slip, until at 870 deg C only the 100 and 011 specimens exhibited normal octahedral slip. The yield strength for octahedral slip was numerically analysed using a model proposed by Lall, Chin, and Pope to explain deviations from Schmid's Law in the yielding behavior of a single phase Gamma prime alloy, Ni3(Al, Nb). The Schmid's Law deviations in Rene N4 were found to be largely due to a tension-compression anisotropy. A second effect, which increases trength for orientations away from 001, was found to be small in Rene N4. Analysis of recently published data on the single crystal superalloy PWA 1480 yielded the same result.

Growth and characterization of CaCu3Ti4O12 single crystals

NASA Astrophysics Data System (ADS)

Kim, Hui Eun; Yang, Sang-don; Lee, Jung-Woo; Park, Hyun Min; Yoo, Sang-Im

2014-12-01

The CaCu3Ti4O12 (CCTO) single crystals could be grown from the melt with the nominal composition of Ca:Cu:Ti=1:59:20 in a platinum (Pt) crucible using a self-flux method. The flux-grown CCTO single crystals have well-developed {100} habit planes, and their compositions are close to the ratio of Ca:Cu:Ti=1:3:4. Interestingly, flux-grown CCTO single crystals exhibited two different back reflection Laue patterns; one exhibited only [100] cubic Laue patterns, and the other showed not only [100] cubic Laue patterns but also the satellite spots related to the twin boundary, implying that twin-free CCTO single crystals can be grown by the self-flux method. Both the dielectric constants and losses of twinned CCTO single crystal are significantly higher than those of untwined CCTO crystal at relatively low frequency regime (<10 kHz), suggesting that the dielectric property is sensitive to the twin boundary.

A multistep single-crystal-to-single-crystal bromodiacetylene dimerization

NASA Astrophysics Data System (ADS)

Hoheisel, Tobias N.; Schrettl, Stephen; Marty, Roman; Todorova, Tanya K.; Corminboeuf, Clémence; Sienkiewicz, Andrzej; Scopelliti, Rosario; Schweizer, W. Bernd; Frauenrath, Holger

2013-04-01

Packing constraints and precise placement of functional groups are the reason that organic molecules in the crystalline state often display unusual physical or chemical properties not observed in solution. Here we report a single-crystal-to-single-crystal dimerization of a bromodiacetylene that involves unusually large atom displacements as well as the cleavage and formation of several bonds. Density functional theory computations support a mechanism in which the dimerization is initiated by a [2 + 1] photocycloaddition favoured by the nature of carbon-carbon short contacts in the crystal structure. The reaction proceeded up to the theoretical degree of conversion without loss of crystallinity, and it was also performed on a preparative scale with good yield. Moreover, it represents the first synthetic pathway to (E)-1,2-dibromo-1,2-diethynylethenes, which could serve as synthetic intermediates for the preparation of molecular carbon scaffolds. Our findings both extend the scope of single-crystal-to-single-crystal reactions and highlight their potential as a synthetic tool for complex transformations.

Preparation of Gd(OH){sub 3} large single crystals by solid KOH assisted hydrothermal method and their luminescent and magnetic properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Hai; Zhang, Youjin, E-mail: zyj@ustc.edu.cn; Zhou, Maozhong

Highlights: • Gd(OH){sub 3} large single crystals were prepared by solid KOH assisted hydrothermal method. • The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. • The Gd(OH){sub 3} samples emitted a strong narrow-band ultraviolet B (NB-UVB) light. • The Gd(OH){sub 3} samples showed good paramagnetic properties. - Abstract: Large single crystals of gadolinium hydroxide [Gd(OH){sub 3}] in the length of several millimeters were successfully prepared by using solid KOH assisted hydrothermal method. Gd(OH){sub 3} samples were characterized by X-ray diffraction (XRD), 4-circle single-crystal diffraction, Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS). FESEM imagemore » shows hexagonal prism morphology for the Gd(OH){sub 3} large crystals. The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. The photoluminescence and magnetic properties of Gd(OH){sub 3} species were investigated.« less

Method for the growth of large low-defect single crystals

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor); Neudeck, Philip G. (Inventor); Trunek, Andrew J. (Inventor); Spry, David J. (Inventor)

2008-01-01

A method and the benefits resulting from the product thereof are disclosed for the growth of large, low-defect single-crystals of tetrahedrally-bonded crystal materials. The process utilizes a uniquely designed crystal shape whereby the direction of rapid growth is parallel to a preferred crystal direction. By establishing several regions of growth, a large single crystal that is largely defect-free can be grown at high growth rates. This process is particularly suitable for producing products for wide-bandgap semiconductors, such as SiC, GaN, AlN, and diamond. Large low-defect single crystals of these semiconductors enable greatly enhanced performance and reliability for applications involving high power, high voltage, and/or high temperature operating conditions.

Crystalline perfection and optical studies of L-Histidinium dihydrogen phosphate orthophosphoric acid (LHDP) single crystals

NASA Astrophysics Data System (ADS)

Ittyachan, Reena; Arunkumar, A.; Bhagavannarayana, G.

2015-10-01

Single crystals of L-Histidinium dihydrogenphosphate orthophosphoric acid (LHDP) were grown by slow evaporation solution growth technique. The grown crystals were confirmed by single crystal X-ray diffraction techniques. The HRXRD rocking curve measurements revealed the crystalline perfection of grown crystal and the absence of structural grain boundaries. The lower optical cut-off wavelength for this crystal was observed at 240 nm. The third order nonlinear refractive index (n2), nonlinear absorption coefficient (β) and susceptibility (χ(3)) were calculated by Z-scan studies using Nd: YAG laser as a source. The single shot laser damage threshold of grown crystal was measured to be 6.286 GW/cm2 using Nd: YAG laser.

A Test of Macromolecular Crystallization in Microgravity: Large, Well-Ordered Insulin Crystals

NASA Technical Reports Server (NTRS)

Borgstahl, Gloria E. O.; Vahedi-Faridi, Ardeschir; Lovelace, Jeff; Bellamy, Henry D.; Snell, Edward H.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

Crystals of insulin grown in microgravity on space shuttle mission STS-95 were extremely well-ordered and unusually large (many > 2 mm). The physical characteristics of six microgravity and six earth-grown crystals were examined by X-ray analysis employing superfine f slicing and unfocused synchrotron radiation. This experimental setup allowed hundreds of reflections to be precisely examined for each crystal in a short period of time. The microgravity crystals were on average 34 times larger, had 7 times lower mosaicity, had 54 times higher reflection peak heights and diffracted to significantly higher resolution than their earth grown counterparts. A single mosaic domain model could account for reflections in microgravity crystals whereas reflections from earth crystals required a model with multiple mosaic domains. This statistically significant and unbiased characterization indicates that the microgravity environment was useful for the improvement of crystal growth and resultant diffraction quality in insulin crystals and may be similarly useful for macromolecular crystals in general.

Gleaming and dull surface textures from photonic-crystal-type nanostructures in the butterfly Cyanophrys remus.

PubMed

Kertész, Krisztián; Bálint, Zsolt; Vértesy, Zofia; Márk, Géza I; Lousse, Virginie; Vigneron, Jean Pol; Rassart, Marie; Biró, László P

2006-08-01

Photonic-crystal-type nanostructures occurring in the scales of the butterfly Cyanophrys remus were investigated by optical and electron microscopy (scanning and transmission electron microscopy), reflectance measurements (specular, integrated, and goniometric), by fast Fourier transform analysis of micrographs, by modeling, and by numerical simulation of the measured reflectance data. By evaluating the collected data in a cross-correlated way, we show that the metallic blue dorsal coloration originates from scales which individually are photonic single crystals of 50 x 120 microm2 , while the matt pea-green coloration of the ventral side arises from the cumulative effect of randomly arranged, bright photonic crystallites (blue, green, and yellow) with typical diameters in the 3-10-mum range. Both structures are based on a very moderate refractive index contrast between air and chitin. Using a bleached specimen in which the pigment has decayed with time, we investigated the role of pigment in photonic-crystal material in the process of color generation. The possible biologic utility of the metallic blue (single-crystal) and dull green (polycrystal) textures both achieved with photonic crystals are briefly discussed. Potential applications in the field of colorants, flat panel displays, smart textiles, and smart papers are surveyed.

Low carrier semiconductor like behavior in Lu3Ir4Ge13 single crystal

NASA Astrophysics Data System (ADS)

Kumar, Anil; Matteppanavar, Shidaling; Thamizhavel, A.; Ramakrishnan, S.

2018-04-01

Single crystal of Lu3Ir4Ge13 crystallizing in the Yb3Rh4Sn13-type cubic crystal structure has been grown by Czochralski method in a tetra-arc furnace. In this paper we report on the crystal structure, magnetic and transport properties of Lu3Ir4Ge13. The analysis of the powder x-ray diffraction (XRD) studies revealed that Lu3Ir4Ge13 crystallizes in a cubic structure with the space group Pm-3n, no. 223. The lattice parameter was obtained from the Rietveld refinement of the room temperature XRD data which amounts to 8.904 (3) Å with low R factors. The temperature dependence of the resistivity exhibited semiconductor like behavior till 1.8 K, with a broad hump around 15 - 62 K. This hump was observed in both warming and cooling cycle with a very small hysteresis, it may be due to the existence of structural transition from high - low symmetry. The temperature dependent magnetization data shows the diamagnetic behavior with an anomaly around 70 K, which is well supported by the derivative of resistivity data.

Resolution extension by image summing in serial femtosecond crystallography of two-dimensional membrane-protein crystals

DOE PAGES

Casadei, Cecilia M.; Tsai, Ching-Ju; Barty, Anton; ...

2018-01-01

Previous proof-of-concept measurements on single-layer two-dimensional membrane-protein crystals performed at X-ray free-electron lasers (FELs) have demonstrated that the collection of meaningful diffraction patterns, which is not possible at synchrotrons because of radiation-damage issues, is feasible. Here, the results obtained from the analysis of a thousand single-shot, room-temperature X-ray FEL diffraction images from two-dimensional crystals of a bacteriorhodopsin mutant are reported in detail. The high redundancy in the measurements boosts the intensity signal-to-noise ratio, so that the values of the diffracted intensities can be reliably determined down to the detector-edge resolution of 4 Å. The results show that two-dimensional serial crystallography atmore » X-ray FELs is a suitable method to study membrane proteins to near-atomic length scales at ambient temperature. The method presented here can be extended to pump–probe studies of optically triggered structural changes on submillisecond timescales in two-dimensional crystals, which allow functionally relevant large-scale motions that may be quenched in three-dimensional crystals.« less

Resolution extension by image summing in serial femtosecond crystallography of two-dimensional membrane-protein crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Casadei, Cecilia M.; Tsai, Ching-Ju; Barty, Anton

Previous proof-of-concept measurements on single-layer two-dimensional membrane-protein crystals performed at X-ray free-electron lasers (FELs) have demonstrated that the collection of meaningful diffraction patterns, which is not possible at synchrotrons because of radiation-damage issues, is feasible. Here, the results obtained from the analysis of a thousand single-shot, room-temperature X-ray FEL diffraction images from two-dimensional crystals of a bacteriorhodopsin mutant are reported in detail. The high redundancy in the measurements boosts the intensity signal-to-noise ratio, so that the values of the diffracted intensities can be reliably determined down to the detector-edge resolution of 4 Å. The results show that two-dimensional serial crystallography atmore » X-ray FELs is a suitable method to study membrane proteins to near-atomic length scales at ambient temperature. The method presented here can be extended to pump–probe studies of optically triggered structural changes on submillisecond timescales in two-dimensional crystals, which allow functionally relevant large-scale motions that may be quenched in three-dimensional crystals.« less

Purification, crystallization and preliminary X-ray diffraction of SecDF, a translocon-associated membrane protein, from Thermus thermophilus

PubMed Central

Tsukazaki, Tomoya; Mori, Hiroyuki; Fukai, Shuya; Numata, Tomoyuki; Perederina, Anna; Adachi, Hiroaki; Matsumura, Hiroyoshi; Takano, Kazufumi; Murakami, Satoshi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo; Vassylyev, Dmitry G.; Nureki, Osamu; Ito, Koreaki

2006-01-01

Thermus thermophilus has a multi-path membrane protein, TSecDF, as a single-chain homologue of Escherichia coli SecD and SecF, which form a translocon-associated complex required for efficient preprotein translocation and membrane-protein integration. Here, the cloning, expression in E. coli, purification and crystallization of TSecDF are reported. Overproduced TSecDF was solubilized with dodecylmaltoside, chromatographically purified and crystallized by vapour diffusion in the presence of polyethylene glycol. The crystals yielded a maximum resolution of 4.2 Å upon X-ray irradiation, revealing that they belonged to space group P43212. Attempts were made to improve the diffraction quality of the crystals by combinations of micro-stirring, laser-light irradiation and dehydration, which led to the eventual collection of complete data sets at 3.74 Å resolution and preliminary success in the single-wavelength anomalous dispersion analysis. These results provide information that is essential for the determination of the three-dimensional structure of this important membrane component of the protein-translocation machinery. PMID:16582489

Crystal structure, vibrational and DFT simulation studies of melaminium dihydrogen phosphite monohydrate

NASA Astrophysics Data System (ADS)

Arjunan, V.; Kalaivani, M.; Marchewka, M. K.; Mohan, S.

2013-08-01

The crystal structure investigations of melamine with phosphorous acid, namely melaminium dihydrogenphosphite monohydrate (C3N6H7·H2PO3·H2O) have been investigated by means of single crystal X-ray diffraction method. The title compound crystallizes in monoclinic crystal system, and the space group is P21/c with a = 10.069 Å, b = 21.592 Å, c = 12.409 Å and Z = 12. The vibrational assignments and analysis of melaminium dihydrogen phosphite monohydrate have also been performed by FTIR, FT-Raman and far-infrared spectral studies. The quantum chemical simulations were performed with DFT (B3LYP) method using 6-31G**, cc-pVTZ, and 6-311++G** basis sets to determine the energy, structural, thermodynamic parameters and vibrational frequencies of melaminium dihydrogen phosphite monohydrate. The hydrogen atom from phosphorous acid was transferred to the melamine molecule giving the singly protonated melaminium cation. The ability of ions to form spontaneous three-dimensional structure through weak Osbnd H···O and Nsbnd H···O hydrogen bonds shows notable vibrational effects.

How far could energy transport within a single crystal

NASA Astrophysics Data System (ADS)

Zhang, Yifan; Che, Yanke; Zhao, Jincai; Steve, Granick

Efficient transport of excitation energy over long distance is a vital process in light-harvesting systems and molecular electronics. The energy transfer distance is largely restricted by the probability decay of the exciton when hopping within a single crystal. Here, we fabricated an organic single crystal within which the energy could transfer more than 100 μm, a distance only limited by its crystal size. Our system could be regarded as a ``Sprint relay game'' performing on different surface of tracks. Photoinduced ``athletes'' (excitons) triggered intermolecular ``domino'' reaction to propagate energy for a long distance. In addition, athletes with the same ability runs much farther on smooth ideal track (single crystal assembled from merely van der Waals interaction) than bumpy mud track (crystal assembled from combination of pi-stacking, hydrogen bond and van der Waals interactions). Our finding presents new physics on enhancing energy transfer length within a single crystal. Current Affiliation: Institute for Basic Science, South Korea.

Single crystal growth by gel technique and characterization of lithium hydrogen tartrate

NASA Astrophysics Data System (ADS)

Ahmad, Nazir; Ahmad, M. M.; Kotru, P. N.

2015-02-01

Single crystal growth of lithium hydrogen tartrate by gel encapsulation technique is reported. Dependence of crystal count on gel density, gel pH, reactant concentration and temperature are studied and the optimum conditions for these crystals are worked out. The stoichiometric composition of the grown crystals is determined using EDAX/AES and CH analysis. The grown crystals are characterized by X-ray diffraction, FTIR and Uv-Visible spectroscopy. It is established that crystal falls under orthorhombic system and space group P222 with the cell parameters as: a=10.971 Å, b=13.125 Å and c=5.101 Å; α=90.5o, β=γ=90°. The morphology of the crystals as revealed by SEM is illustrated. Crystallite size, micro strain, dislocation density and distortion parameters are calculated from the powder XRD results of the crystal. UV-vis spectroscopy shows indirect allowed transition with an optical band gap of 4.83 eV. The crystals are also shown to have high transmittance in the entire visible region. Dependence of dielectric constant, dielectric loss and conductivity on frequency of the applied ac field is analyzed. The frequency-dependent real part of the complex ac conductivity is found to follow the universal dielectric response: σac (ω) ωs. The trend in the variation of frequency exponent with frequency corroborates the fact that correlated barrier hopping is the dominant charge-transport mechanism in the present system.

Facile synthesis, single crystal analysis, and computational studies of sulfanilamide derivatives

NASA Astrophysics Data System (ADS)

Tahir, Muhammad Nawaz; Khalid, Muhammad; Islam, Ayesha; Ali Mashhadi, Syed Muddassir; Braga, Ataualpa A. C.

2017-01-01

Antibacterial resistance is a worldwide problem. Sulfanilamide is widely used antibacterial. For the first time, we report here a simple method for the derivative synthesis of the title drugs, single crystal XRD and density functional theory (DFT) studies. The optimized molecular structure, natural bond orbital (NBO), frontier molecular orbitals (FMOs) molecular electrostatic potential studies (MEP) and Mulliken population analysis (MPA) have been performed using M06-2X/6-31G(d, p). The FT-IR spectra and thermodynamic parameters were calculated at M06-2X/6-311 + G(2d,p) and B3LYP/6-31G(d, p) levels respectively, while, the UV-Vis analysis was performed using TD-DFT/B3LYP/6-31G(d, p) method. The experimental FT-IR spectra of both compounds were also carried out to reconfirm sbnd H⋯Osbnd hydrogen bonds. The DFT optimized parameters exhibiting good agreement with the experimental data. NBO analysis explored the hyper conjugative interaction and stability of title crystals, especially, reconfirmed the existence of sbnd H⋯Osbnd hydrogen bonds between the dimers. The FT-IR, thermodynamic parameters, MEP and MPA also revealed the hydrogen bonding detail is harmonious to XRD data. As a matter of the fact, the hydrogen bonding is a significant parameter for the understanding and design of molecular crystals, subsequently; it can also play a vital role in the supramolecular chemistry. Moreover, the global reactivity descriptors suggest that title compounds might be bioactive.

Crystal growth and molecular modeling studies of inhibition of struvite by phosphocitrate.

PubMed

Wierzbicki, A; Sallis, J D; Stevens, E D; Smith, M; Sikes, C S

1997-09-01

The inhibition by phosphocitrate of struvite crystal formation and growth has been examined in the present study. Crystal growth in a gel matrix was controlled by phosphocitrate in a dose-dependent manner. The effects of inhibition were followed using scanning electron microscopy, optical microscopy, and single crystal X-ray analysis. The presence of phosphocitrate induced very strong, crystal face specific inhibition of struvite, leading to total cessation of crystal growth when sufficient concentration of the inhibitor was made available. Crystal growth studies and results from molecular modeling indicated strong affinity of phosphocitrate to (101) faces of struvite. This in turn led to an alteration in the expression of these faces and the development of a characteristic arrowhead struvite morphology. Similar changes were not observed in the presence of identical concentrations of citrate, acetohydroxamic acid, and N-sulfo-2 amino tricarballylate (an analog of phosphocitrate), emphasizing the unique interaction of phosphocitrate with the struvite crystal lattice.

Magnetic interactions and magnetic anisotropy in exchange coupled 4f-3d systems: a case study of a heterodinuclear Ce3+-Fe3+ cyanide-bridged complex.

PubMed

Sorace, Lorenzo; Sangregorio, Claudio; Figuerola, Albert; Benelli, Cristiano; Gatteschi, Dante

2009-01-01

We report here a detailed single-crystal EPR and magnetic study of a homologous series of complexes of the type Ln-M (Ln = La(III), Ce(III); M = Fe(III), Co(III)). We were able to obtain a detailed picture of the low-lying levels of Ce(III) and Fe(III) centres through the combined use of single-crystal EPR and magnetic susceptibility data. We show that classical ligand field theory can be of great help in rationalising the energies of the low-lying levels of both the transition-metal and rare-earth ions. The combined analysis of single-crystal EPR and magnetic data of the coupled system Ce-Fe confirmed the great complexity of the interactions involving rare-earth elements. With little uncertainty, it turned out clearly that the description of the interaction involving the lowest lying spin levels requires the introduction of the isotropic, anisotropic and antisymmetric terms.

Synthesis, spectral, structural prediction and computational studies of octylcarbazole ornamented 3-phenothiazinal

NASA Astrophysics Data System (ADS)

Karuppasamy, Ayyanar; Udhaya kumar, Chandran; Karthikeyan, Subramanian; Velayutham Pillai, Muthiah Pillai; Ramalingan, Chennan

2017-11-01

A novel conjugated octylcarbazole ornamented 3-phenothiazinal, 10-(9-octyl-9H-carbazol-3-yl)-10H-phenothiazine-3-carbaldehyde (OCPTC) was synthesized and fully characterized by 1H-NMR, 13C-NMR, elemental and single crystal XRD analyses. The optimized geometrical structure, vibrational frequencies and NMR have been computed with M06-2X method using 6-31+G(d,p) basis set. Total electronic energies and HOMO-LUMO energy gaps in gas phase are discussed. The geometrical parameters of the title compound obtained from single crystal XRD studies have been found in accord with the calculated (DFT) values. The experimental and theoretical FT-IR and NMR results of the title molecule have been investigated. The experimentally observed vibrational frequencies have been compared with the calculated ones, which are in good agreement with each other. Single crystal X-ray structural analysis of OCPTC, evidences the ''butterfly conformation'' of phenothiazine ring with nearly perpendicular orientation of the carbazole structural motif to the phenothiazine moiety.

Studies on the self-catalyzed Knoevenagel condensation, characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques

NASA Astrophysics Data System (ADS)

Suresh Kumar, G. S.; Antony Muthu Prabhu, A.; Bhuvanesh, N.

2014-10-01

We have studied the self-catalyzed Knoevenagel condensation, spectral characterization, DPPH radical scavenging activity, cytotoxicity, and molecular properties of 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones using single crystal XRD and DFT techniques. In the absence of any catalyst, a series of novel 5-arylidene-2,2-dimethyl-1,3-dioxane-4,6-diones were synthesized using Meldrum’s acid and formylphenoxyaliphatic acid(s) in water. These molecules are arranged in the dimer form through intermolecular H-bonding in the single crystal XRD structure. Compounds have better DPPH radical scavenging activity and cytotoxicity against A431 cancer cell line. The optimized molecular structure, natural bond orbital analysis, electrostatic potential map, HOMO-LUMO energies, molecular properties, and atomic charges of these molecules have been studied by performing DFT/B3LYP/3-21G(*) level of theory in gas phase.

Predicting Catalytic Activity of Nanoparticles by a DFT-Aided Machine-Learning Algorithm.

PubMed

Jinnouchi, Ryosuke; Asahi, Ryoji

2017-09-07

Catalytic activities are often dominated by a few specific surface sites, and designing active sites is the key to realize high-performance heterogeneous catalysts. The great triumphs of modern surface science lead to reproduce catalytic reaction rates by modeling the arrangement of surface atoms with well-defined single-crystal surfaces. However, this method has limitations in the case for highly inhomogeneous atomic configurations such as on alloy nanoparticles with atomic-scale defects, where the arrangement cannot be decomposed into single crystals. Here, we propose a universal machine-learning scheme using a local similarity kernel, which allows interrogation of catalytic activities based on local atomic configurations. We then apply it to direct NO decomposition on RhAu alloy nanoparticles. The proposed method can efficiently predict energetics of catalytic reactions on nanoparticles using DFT data on single crystals, and its combination with kinetic analysis can provide detailed information on structures of active sites and size- and composition-dependent catalytic activities.

Acoustic emission evolution during sliding friction of Hadfield steel single crystal

NASA Astrophysics Data System (ADS)

Lychagin, D. V.; Novitskaya, O. S.; Kolubaev, A. V.; Sizova, O. V.

2017-12-01

Friction is a complex dynamic process. Direct observation of processes occurring in the friction zone is impossible due to a small size of a real contact area and, as a consequence, requires various additional methods applicable to monitor a tribological contact state. One of such methods consists in the analysis of acoustic emission data of a tribological contact. The use of acoustic emission entails the problem of interpreting physical sources of signals. In this paper, we analyze the evolution of acoustic emission signal frames in friction of Hadfield steel single crystals. The chosen crystallographic orientation of single crystals enables to identify four stages related to friction development as well as acoustic emission signals inherent in these stages. Acoustic emission signal parameters are studied in more detail by the short-time Fourier transform used to determine the time variation of the median frequency and its power spectrum. The results obtained will facilitate the development of a more precise method to monitor the tribological contact based on the acoustic emission method.

Synthesis, optical, experimental and theoretical investigation of third order nonlinear optical properties of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

Bharathi, M. Divya; Bhuvaneswari, R.; Srividya, J.; Vinitha, G.; Prithiviraajan, R. N.; Anbalagan, G.

2018-02-01

Single crystals of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate (8HQNP) were obtained from slow evaporation solution growth method using methanol-water (1:1) as a solvent. Powder X-ray diffraction was utilized to compute the unit cell parameters and dislocation density of 8HQNP crystal. The crystalline perfection of the as-grown crystal was investigated by high-resolution X-ray diffraction at room temperature. The molecular structure was analyzed by identifying the functional groups from FT-IR and FT-Raman spectra. The cut-off wavelength and the corresponding optical band gap obtained from an optical spectrum were 376 nm and 3.29 eV respectively. The dispersion nature of refractive index was investigated by the single-oscillator Wemple and Di-Domenico model. Red emission was observed in the photoluminescence spectrum when excited with 376 nm. The low birefringence and high laser damage threshold (8.538 GW/cm2) values dictate the suitability of the crystal for optical devices. Z-scan studies revealed the third order nonlinear absorption coefficient (β) and refractive index (n2) of the 8HQNP crystal. The theoretical value of third order nonlinear susceptibility obtained from density function theory is good accordance with the experimental value. The frontier molecular orbital energy gap decreases with increasing external electric field in different directions which attributed to the enhancement of the second hyperpolarizability. The grown title crystal is thermally stable up to 102 °C which was identified using thermal analysis. Mechanical strength of 8HQNP was estimated by using Vicker's microhardness studies.

Analysis of the convergence rules of full-range PSD surface error of magnetorheological figuring KDP crystal.

PubMed

Chen, Shaoshan; He, Deyu; Wu, Yi; Chen, Huangfei; Zhang, Zaijing; Chen, Yunlei

2016-10-01

A new non-aqueous and abrasive-free magnetorheological finishing (MRF) method is adopted for processing potassium dihydrogen phosphate (KDP) crystal due to its low hardness, high brittleness, temperature sensitivity, and water solubility. This paper researches the convergence rules of the surface error of an initial single-point diamond turning (SPDT)-finished KDP crystal after MRF polishing. Currently, the SPDT process contains spiral cutting and fly cutting. The main difference of these two processes lies in the morphology of intermediate-frequency turning marks on the surface, which affects the convergence rules. The turning marks after spiral cutting are a series of concentric circles, while the turning marks after fly cutting are a series of parallel big arcs. Polishing results indicate that MRF polishing can only improve the low-frequency errors (L>10  mm) of a spiral-cutting KDP crystal. MRF polishing can improve the full-range surface errors (L>0.01  mm) of a fly-cutting KDP crystal if the polishing process is not done more than two times for single surface. We can conclude a fly-cutting KDP crystal will meet better optical performance after MRF figuring than a spiral-cutting KDP crystal with similar initial surface performance.

Linear electro-optic properties of relaxor-based ferroelectric 0.24Pb(In1/2Nb1/2)O3-(0.76 − x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 single crystals

PubMed Central

Wu, Fengmin; Yang, Bin; Sun, Enwei; Liu, Gang; Tian, Hao; Cao, Wenwu

2013-01-01

Linear electro-optic properties of 0.24Pb(In1/2Nb1/2)O3-(0.76 − x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 single crystals, with compositions in the rhombohedral, morphotropic phase boundary (MPB) and tetragonal phases, have been investigated. Very large effective electro-optic coefficient γc (204 pm/V) was observed in a crystal with the MPB composition when it is poled along [001]. The rhombohedral phase (x = 0.27 and 0.30) single crystals poled along [111] direction and tetragonal phase (x = 0.39) single crystal poled along [001] direction are in single domain, and their electro-optic coefficients (γc = 76, 94, and 43 pm/V for the crystals with x = 0.27, 0.30, and 0.39, respectively) were found to be much higher than that of traditional electro-optic single crystal LiNbO3 (γc = 19.9 pm/V). The electro-optic coefficients of the single crystal in the rhombohedral phase have excellent temperature stability in the experimental temperature range of 10–40 °C. The half-wave voltage Vπ was calculated to be much lower (less than 1000 V) than that of LiNbO3 single crystal (2800 V). These superior properties make the ternary relaxor-PT single crystals very promising for electro-optic modulation applications. PMID:23922449

Single crystal and optical ceramic multicomponent garnet scintillators: A comparative study

NASA Astrophysics Data System (ADS)

Wu, Yuntao; Luo, Zhaohua; Jiang, Haochuan; Meng, Fang; Koschan, Merry; Melcher, Charles L.

2015-04-01

Multicomponent garnet materials can be made in optical ceramic as well as single crystal form due to their cubic crystal structure. In this work, high-quality Gd3Ga3Al2O12:0.2 at% Ce (GGAG:Ce) single crystal and (Gd,Lu)3Ga3Al2O12:1 at% Ce (GLuGAG:Ce) optical ceramics were fabricated by the Czochralski method and a combination of hot isostatic pressing (HIPing) and annealing treatment, respectively. Under optical and X-ray excitation, the GLuGAG:Ce optical ceramic exhibits a broad Ce3+ transition emission centered at 550 nm, while the emission peak of the GGAG:Ce single crystal is centered at 540 nm. A self-absorption effect in GLuGAG:Ce optical ceramic results in this red-shift of the Ce3+ emission peak compared to that in the GGAG:Ce single crystal. The light yield under 662 keV γ-ray excitation was 45,000±2500 photons/MeV and 48,200±2410 photons/MeV for the GGAG:Ce single crystal and GLuGAG:Ce optical ceramic, respectively. An energy resolution of 7.1% for 662 keV γ-rays was achieved in the GLuGAG:Ce optical ceramic with a Hamamatsu R6231 PMT, which is superior to the value of 7.6% for a GGAG:Ce single crystal. Scintillation decay time measurements under 137Cs irradiation show two exponential decay components of 58 ns (47%) and 504 ns (53%) for the GGAG:Ce single crystal, and 84 ns (76%) and 148 ns (24%) for the GLuGAG:Ce optical ceramic. The afterglow level after X-ray cutoff in the GLuGAG:Ce optical ceramic is at least one order of magnitude lower than in the GGAG:Ce single crystal.

Elastic response of (001)-oriented PWA 1480 single crystal - The influence of secondary orientation

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Azis, Ali; Mcgaw, Michael

1991-01-01

The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

Method of making single crystal fibers

NASA Technical Reports Server (NTRS)

Westfall, Leonard J. (Inventor)

1990-01-01

Single crystal fibers are made from miniature extruded ceramic feed rods. A decomposable binder is mixed with powders to inform a slurry which is extruded into a small rod which may be sintered, either in air or in vacuum, or it may be used in the extruded and dried condition. A pair of laser beams focuses onto the tip of the rod to melt it thereby forming a liquid portion. A single crystal seed fiber of the same material as the feed rod contacts this liquid portion to establish a zone of liquid material between the feed rod and the single crystal seed fiber. The feed rod and the single crystal feed fiber are moved at a predetermined speed to solidify the molten zone onto the seed fiber while simultaneously melting additional feed rod. In this manner a single crystal fiber is formed from the liquid portion.

Distributed Feedback Laser Based on Single Crystal Perovskite

NASA Astrophysics Data System (ADS)

Sun, Shang; Xiao, Shumin; Song, Qinghai

2017-06-01

We demonstrate a single crystal perovskite based, with grating-structured photoresist on top, highly polarized distributed feedback laser. A lower laser threshold than the Fabry-Perot mode lasers from the same single crystal CH3NH3PbBr3 microplate was obtained. Single crystal CH3NH3PbBr3 microplates was synthesized with one-step solution processed precipitation method. Once the photoresist on top of the microplate was patterned with electron beam, the device was realized. This one-step fabrication process utilized the advantage of single crystal to the greatest extend. The ultra-low defect density in single crystalline microplate offer an opportunity for lower threshold lasing action compare with poly-crystal perovskite films. In the experiment, the lasing action based on the distributed feedback grating design was found with lower threshold and higher intensity than the Fabry-Perot mode lasers supported by the flat facets of the same microplate.

Effect of grain boundary on the field-effect mobility of microrod single crystal organic transistors.

PubMed

Kim, Jaekyun; Kang, Jingu; Cho, Sangho; Yoo, Byungwook; Kim, Yong-Hoon; Park, Sung Kyu

2014-11-01

High-performance microrod single crystal organic transistors based on a p-type 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) semiconductor are fabricated and the effects of grain boundaries on the carrier transport have been investigated. The spin-coating of C8-BTBT and subsequent solvent vapor annealing process enabled the formation of organic single crystals with high aspect ratio in the range of 10 - 20. It was found that the organic field-effect transistors (OFETs) based on these single crystals yield a field-effect mobility and an on/off current ratio of 8.04 cm2/Vs and > 10(5), respectively. However, single crystal OFETs with a kink, in which two single crystals are fused together, exhibited a noticeable drop of field-effect mobility, and we claim that this phenomenon results from the carrier scattering at the grain boundary.

Single crystal diamond membranes for nanoelectronics.

PubMed

Bray, Kerem; Kato, Hiromitsu; Previdi, Rodolfo; Sandstrom, Russell; Ganesan, Kumaravelu; Ogura, Masahiko; Makino, Toshiharu; Yamasaki, Satoshi; Magyar, Andrew P; Toth, Milos; Aharonovich, Igor

2018-02-22

Single crystal, nanoscale diamond membranes are highly sought after for a variety of applications including nanophotonics, nanoelectronics and quantum information science. However, so far, the availability of conductive diamond membranes has remained an unreachable goal. In this work we present a complete nanofabrication methodology for engineering high aspect ratio, electrically active single crystal diamond membranes. The membranes have large lateral directions, exceeding ∼500 × 500 μm 2 and are only several hundreds of nanometers thick. We further realize vertical single crystal p-n junctions made from the diamond membranes that exhibit onset voltages of ∼10 V and a current of several mA. Moreover, we deterministically introduce optically active color centers into the membranes, and demonstrate for the first time a single crystal nanoscale diamond LED. The robust and scalable approach to engineer the electrically active single crystal diamond membranes offers new pathways for advanced nanophotonic, nanoelectronic and optomechanical devices employing diamond.

The effect of Fe 3+ doping in Potassium Hydrogen Phthalate single crystals on structural and optical properties

NASA Astrophysics Data System (ADS)

Kumar, R. Ashok; Sivakumar, N.; Vizhi, R. Ezhil; Babu, D. Rajan

2011-02-01

This work investigates the influence of iron doping on Potassium Hydrogen Phthalate (KHP) single crystals by the slow evaporation solution growth technique. Factors such as evaporation rate, solution pH, solute concentration, super saturation limit, etc. are very important in order to have optically transparent single crystals. As part of the work, the effects of metallic salt FeCl 3 in different concentrations were analyzed with pure KHP. Powder X-ray diffraction suggests that the grown crystals are crystallized in the orthorhombic structure. The functional groups and the effect of moisture on the doped crystals can be analyzed with the help of a FTIR spectrum. The pure and doped KHP single crystal shows good transparency in the entire visible region, which is suitable for optical device applications. The refractive indices along b axis of pure and doped KHP single crystals were analyzed by the prism coupling technique. The emission of green light with the use of a Nd:YAG laser ( λ=1064 nm) confirmed the second harmonic generation properties of the grown crystals.

Crystallization of the collagen-like polypeptide (PPG)10 aboard the International Space Station. 1. Video observation.

PubMed

Vergara, Alessandro; Corvino, Ermanno; Sorrentino, Giosué; Piccolo, Chiara; Tortora, Alessandra; Carotenuto, Luigi; Mazzarella, Lelio; Zagari, Adriana

2002-10-01

Single chains of the collagen model polypeptide with sequence (Pro-Pro-Gly)(10), hereafter referred to as (PPG)(10), aggregate to form rod-shaped triple helices. Crystals of (PPG)(10) were grown in the Advanced Protein Crystallization Facility (APCF) both onboard the International Space Station (ISS) and on Earth. The experiments allow the direct comparison of four different crystallization environments for the first time: solution in microgravity ((g), agarose gel in (g, solution on earth, and gel on earth. Both on board and on ground, the crystal growth was monitored by a CCD video camera. The image analysis provided information on the spatial distribution of the crystals, their movement and their growth rate. The analysis of the distribution of crystals reveals that the crystallization process occurs as it does in batch conditions. Slow motions have been observed onboard the ISS. Different to Space-Shuttle experiment, the crystals onboard the ISS moved coherently and followed parallel trajectories. Growth rate and induction time are very similar both in gel and in solution, suggesting that the crystal growth rate is controlled by the kinetics at the interface under the used experimental conditions. These results provide the first data in the crystallogenesis of (PPG)(10), which is a representative member of non-globular, rod-like proteins.

2Flux growth and characterization of Ce-substituted Nd 2 Fe 14 B single crystals

DOE PAGES

Susner, Michael A.; Conner, Benjamin S.; Saparov, Bayrammurad I.; ...

2016-10-27

Single crystals of (Nd 1-xCe x) 2Fe 14B are grown out of Fe-(Nd,Ce) flux. Chemical and structural analysis of the crystals indicate that (Nd 1-xCe x) 2Fe 14B forms a solid solution until at least x = 0.38 with a Vegard-like variation of the lattice constants with x. Refinements of single crystal neutron diffraction data indicate that Ce has a slight site preference (7:3) for the 4g rare earth site over the 4f site. Magnetization measurements at 300 K show only small decreases with increasing Ce content in saturation magnetization (M s) and anisotropy field (H A), and Curie temperaturemore » (T C). First principles calculations are carried out to understand the effect of Ce substitution on the electronic and magnetic properties. For a multitude of applications, it is expected that the advantage of incorporating lower-cost and more abundant Ce will outweigh the small adverse effects on magnetic properties. In conclusion, Ce-substituted Nd 2Fe 14B is therefore a potential high-performance permanent magnet material with substantially reduced Nd content.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sanctis, Daniele de; Rêgo, Ana T.; Marçal, David

The sorbitol operon regulator from K. pneumoniae has been overexpressed in E. coli, purified and crystallized. Diffraction data were collected to 3.2 Å. The sorbitol operon regulator (SorC) regulates the metabolism of l-sorbose in Klebsiella pneumonia. SorC was overexpressed in Escherichia coli and purified, and crystals were obtained of a tetrameric form. A single crystal showed X-ray diffraction to 3.20 Å. The crystal belongs to space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 91.6, b = 113.3, c = 184.1 Å. Analysis of the molecular-replacement solution indicates the presence of four SorC molecules in the asymmetric unit.

Crystallization and preliminary X-ray analysis of a complex formed between the antibiotic simocyclinone D8 and the DNA breakage–reunion domain of Escherichia coli DNA gyrase

PubMed Central

Edwards, Marcus J.; Flatman, Ruth H.; Mitchenall, Lesley A.; Stevenson, Clare E. M.; Maxwell, Anthony; Lawson, David M.

2009-01-01

Crystals of a complex formed between the 59 kDa N-terminal fragment of the Escherichia coli DNA gyrase A subunit (also known as the breakage–reunion domain) and the antibiotic simocyclinone D8 were grown by vapour diffusion. The complex crystallized with I-centred orthorhombic symmetry and X-ray data were recorded to a resolution of 2.75 Å from a single crystal at the synchrotron. DNA gyrase is an essential bacterial enzyme and thus represents an attractive target for drug development. PMID:19652356

Optical properties of bulk gallium nitride single crystals grown by chloride-hydride vapor-phase epitaxy

NASA Astrophysics Data System (ADS)

Agyekyan, V. F.; Borisov, E. V.; Serov, A. Yu.; Filosofov, N. G.

2017-12-01

A gallium nitride crystal 5 mm in thickness was grown by chloride-hydride vapor-phase epitaxy on a sapphire substrate, from which the crystal separated during cooling. At an early stage, a three-dimensional growth mode was implemented, followed by a switch to a two-dimensional mode. Spectra of exciton reflection, exciton luminescence, and Raman scattering are studied in several regions characteristic of the sample. Analysis of these spectra and comparison with previously obtained data for thin epitaxial GaN layers with a wide range of silicon doping enabled conclusions about the quality of the crystal lattice in these characteristic regions.

Growth and characterisation of a new polymorph of barium maleate: a metal organic framework.

PubMed

Nair, Lekshmi P; Bijini, B R; Prasanna, S; Eapen, S M; Nair, C M K; Deepa, M; RajendraBabu, K

2015-02-25

A new polymorph of barium maleate (BM) with chemical formula C24H14O24Ba5⋅7H2O is grown by modified gel method. Transparent plate like crystals of dimensions 9×4×1 mm(3) were obtained. Single crystal X-ray Diffraction analysis was done to determine the structure and the crystal belongs to triclinic system, P-1 space group with cell dimensions a=7.2929(3) Å, b=10.5454(4) Å, c=14.2837(6) Å, α=102.0350(10)°, β=99.1580(10)°, γ=102.9170(10)°. Hydrogen bonding stabilises the two dimensional polymeric crystal structure. Fourier Transform Infrared spectroscopic method was utilised for the analysis of various functional groups present in the complex. Elemental analysis confirmed the stoichiometry of the complex. Thermal properties of the crystal were studied by TGA/DTA. The material melts at 368°C. The optical transparency of the crystal was studied using UV-Visible absorption spectra. The optical band gap is found to be 3.35 eV. Copyright © 2014 Elsevier B.V. All rights reserved.

Tunable top-down fabrication and functional surface coating of single-crystal titanium dioxide nanostructures and nanoparticles

NASA Astrophysics Data System (ADS)

Ha, Seungkyu; Janissen, Richard; Ussembayev, Yera Ye.; van Oene, Maarten M.; Solano, Belen; Dekker, Nynke H.

2016-05-01

Titanium dioxide (TiO2) is a key component of diverse optical and electronic applications that exploit its exceptional material properties. In particular, the use of TiO2 in its single-crystalline phase can offer substantial advantages over its amorphous and polycrystalline phases for existing and yet-to-be-developed applications. However, the implementation of single-crystal TiO2 has been hampered by challenges in its fabrication and subsequent surface functionalization. Here, we introduce a novel top-down approach that allows for batch fabrication of uniform high-aspect-ratio single-crystal TiO2 nanostructures with targeted sidewall profiles. We complement our fabrication approach with a functionalization strategy that achieves dense, uniform, and area-selective coating with a variety of biomolecules. This allows us to fabricate single-crystal rutile TiO2 nanocylinders tethered with individual DNA molecules for use as force- and torque-transducers in an optical torque wrench. These developments provide the means for increased exploitation of the superior material properties of single-crystal TiO2 at the nanoscale.Titanium dioxide (TiO2) is a key component of diverse optical and electronic applications that exploit its exceptional material properties. In particular, the use of TiO2 in its single-crystalline phase can offer substantial advantages over its amorphous and polycrystalline phases for existing and yet-to-be-developed applications. However, the implementation of single-crystal TiO2 has been hampered by challenges in its fabrication and subsequent surface functionalization. Here, we introduce a novel top-down approach that allows for batch fabrication of uniform high-aspect-ratio single-crystal TiO2 nanostructures with targeted sidewall profiles. We complement our fabrication approach with a functionalization strategy that achieves dense, uniform, and area-selective coating with a variety of biomolecules. This allows us to fabricate single-crystal rutile TiO2 nanocylinders tethered with individual DNA molecules for use as force- and torque-transducers in an optical torque wrench. These developments provide the means for increased exploitation of the superior material properties of single-crystal TiO2 at the nanoscale. Electronic supplementary information (ESI) available: Experimental details (ESI Methods) of the optic axis orientation of TiO2 nanocylinders, Cr etch mask fabrication, surface functionalization and its evaluation using fluorescence microscopy, preparation of DNA constructs, assembly of flow cells, bioconjugation of TiO2 nanocylinders, OTW instrumentation and measurements; TiO2 dry etching optimization and the etching parameters employed (Tables S1 and S2); dimensional analysis of TiO2 nanocylinders (Table S3); diverse applications of TiO2 at the nanoscale (Fig. S1); selection of etch mask material (Fig. S2); control of sidewall profiles in TiO2 etching (Fig. S3); size distributions of TiO2 nanocylinders (Fig. S4); quantitative comparisons of different surface linker molecules (Fig. S5); DLS measurements on TiO2 nanocylinders (Fig. S6); optical trap calibration (Fig. S7); and supplementary references. See DOI: 10.1039/c6nr00898d

Influence of tartaric acid on linear-nonlinear optical and electrical properties of KH2PO4 crystal

NASA Astrophysics Data System (ADS)

Baig, M. I.; Anis, Mohd; Muley, G. G.

2017-10-01

KH2PO4 (KDOP) is widely demanded technological crystal for applications in laser driven photonic devices. Therefore, present article is focused to investigate the effect of tartaric acid (TA) on laser induced nonlinear optical properties of KDOP crystal. The optically transparent TA doped KDOP crystal of size 15 × 10 × 04 mm3 has been grown by slow solvent evaporation technique at 35 °C. The structural analysis of pure and TA doped KDOP crystal has been achieved by means of single crystal X-ray diffraction technique. The functional groups of TA doped KDOP crystal has been identified by means of Fourier transform infrared spectral analysis. The UV-visible studies have been performed to determine the optical transparency and evaluate the linear optical constants of pure and TA doped KDOP crystal. The Kurtz-Perry test has been employed to confirm the frequency doubling phenomenon of crystal and the SHG efficiency of TA doped KDOP crystal is found to be 5.68 times higher than that of standard KDP material. The Z-scan technique has been employed to explore the third order nonlinear optical (TONLO) refraction (n2), absorption (β) and susceptibility (χ3) of pure and TA doped KDOP crystal at 632.8 nm. The TA facilitated optical switching in TONLO response of KDOP crystal is found to be an interesting effect to examine. The laser damage threshold of TA doped KDOP crystal has been determined at 1064 nm using the Nd:YAG laser. The comparative electrical analysis on pure and TA doped KDOP crystal has been accomplished by means of dielectric and photoconductivity characterization studies.

Synthesis and characterization of a novel schiff base of 1,2-diaminopropane with substituted salicyaldehyde and its transition metal complexes: Single crystal structures and biological activities

NASA Astrophysics Data System (ADS)

Tadavi, Samina K.; Yadav, Abhijit A.; Bendre, Ratnamala S.

2018-01-01

A novel schiff base H2L derived from simple condensation of 2-hydroxy-6-isopropyl-3-methyl benzaldehyde and 1,2-diaminopropane in 2:1 M ratio and its [MnL], [CoL] and [NiL]2 complexes have been prepared and characterized by spectroscopic technique, elemental analysis, SEM-EDX analysis, and cyclic voltammetry. Additionally, single crystal X-ray diffraction technique has been applied to the schiff base ligand H2L and its nickel complex. The structure of nickel complex exhibited dimeric form with formula [NiL]2 with distorted square planar geometry around each nickel center. Furthermore, all the synthesized compounds were screened for their antimicrobial and antioxidant and DNA cleavage activities.

Method and apparatus for conducting structural health monitoring in a cryogenic, high vibration environment

NASA Technical Reports Server (NTRS)

Qing, Xinlin (Inventor); Beard, Shawn J. (Inventor); Li, Irene (Inventor)

2013-01-01

Sensors affixed to various such structures, where the sensors can withstand, remain affixed, and operate while undergoing both cryogenic temperatures and high vibrations. In particular, piezoelectric single crystal transducers are utilized, and these sensors are coupled to the structure via a low temperature, heat cured epoxy. This allows the transducers to monitor the structure while the engine is operating, even despite the harsh operating conditions. Aspects of the invention thus allow for real time monitoring and analysis of structures that operate in conditions that previously did not permit such analysis. A further aspect of the invention relates to use of piezoelectric single crystal transducers. In particular, use of such transducers allows the same elements to be used as both sensors and actuators.

Growth and properties of oxygen- and ion-doped Bi2Sr2CaCu2O8+δ single crystals

NASA Astrophysics Data System (ADS)

Mitzi, D. B.; Lombardo, L. W.; Kapitulnik, A.; Laderman, S. S.; Jacowitz, R. D.

1990-04-01

A directional solidification method for growing large single crystals in the Bi2Sr2CaCu2O8+δ system is reported. Ion doping, with replacement of La for Sr and Y for Ca, as well as oxygen doping in these crystals has been explored. Doped and undoped crystals have been characterized using microprobe analysis, x-ray diffraction, thermogravimetric analysis, and magnetic and Hall measurements. Ion doping results in little change of the superconducting transition for substitution levels below 20-25%, while beyond this level the Meissner signal broadens and the low-temperature Meissner signal decreases. Microprobe analysis and x-ray diffraction performed on these more highly substituted single crystals provide evidence for inhomogeneity and phase segregation into regions of distinct composition. Annealing unsubstituted crystals in increasing partial pressures of oxygen reversibly depresses the superconducting transition temperature from 90 (as made) to 77 K (oxygen pressure annealed), while the carrier concentrations, as determined from Hall effect measurements, increase from n=3.1(3)×1021 cm-3 (0.34 holes per Cu site) to 4.6(3)×1021 cm-3 (0.50 holes per Cu site). No degradation of the Meissner transition or other indications of inhomogeneity or phase segregation with doping are noted, suggesting that oxygen-doped Bi2Sr2CaCu2O8+δ is a suitable system for pursuing doping studies. The decrease in Tc with concentration for 0.34<=n<=0.50 indicates that a high-carrier-concentration regime exists in which Tc decreases with n and suggests that this decrease does not arise from material inhomogeneity or other materials problems. An examination of the variation of Tc with the density of states and lattice constants for all of the doped and undoped superconducting samples considered here indicates that changes in Tc with doping are primarily affected by changes in the density of states (or carrier concentration) rather than by structural variation induced by the doping.

Selectivity analysis of an incoherent grating imaged in a photorefractive crystal

NASA Astrophysics Data System (ADS)

Tebaldi, Myrian; Forte, Gustavo; Bolognini, Nestor; Lasprilla A., Maria del Carmen

2018-04-01

In this work, the diffraction efficiency of a volume phase grating incoherently stored in a photorefractive BSO crystal is theoretically and experimentally analyzed. The results confirm the theoretical proposal based on the coupled wave theory adopting a new grating depth parameter associated to the write-in incoherent optical system. The selectivity behavior is governed by the exit pupil diameter of the imaging recording system that controls the depth of the tridimensional image distribution along the propagation direction. Two incoherent gratings are multiplexed in a single crystal and reconstructed without cross-talk.

Synthesis, crystal structure and magnetic properties of a novel tetranuclear oxo-bridged iron(III) butterfly

NASA Astrophysics Data System (ADS)

Arizaga, Livia; Gancheff, Jorge S.; Faccio, Ricardo; Cañón-Mancisidor, Walter; González, Ricardo; Kremer, Carlos; Chiozzone, Raúl

2014-01-01

A novel carboxylate/picolinate oxo-bridged iron(III) cluster, namely [Na2(H2O)8][Fe4(μ-O)2(O2CPh)7(pic)2]2·2H2O (1) where pic = picolinate, has been obtained by reacting "basic iron benzoate" [Fe3O(O2CPh)6(H2O)3](O2CPh) with sodium picolinate in acetonitrile. The compound has been characterized by elemental analysis and IR spectroscopy and its crystal structure has been determined by single-crystal X-ray diffraction.

New Polymorph Form of Dexamethasone Acetate.

PubMed

Silva, Ronaldo Pedro da; Ambrósio, Mateus Felipe Schuchter; Piovesan, Luciana Almeida; Freitas, Maria Clara Ramalho; Aguiar, Daniel Lima Marques de; Horta, Bruno Araújo Cautiero; Epprecht, Eugenio Kahn; San Gil, Rosane Aguiar da Silva; Visentin, Lorenzo do Canto

2018-02-01

A new monohydrated polymorph of dexamethasone acetate was crystallized and its crystal structure characterized. The different analytical techniques used for describing its structural and vibrational properties were: single crystal and polycrystal X-ray diffraction, solid state nuclear magnetic resonance, infrared spectroscopy. A Hirshfeld surface analysis was carried out through self-arrangement cemented by H-bonds observed in this new polymorph. This new polymorph form appeared because of self-arrangement via classical hydrogen bonds around the water molecule. Copyright © 2018 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Averaging of elastic constants for polycrystals

DOE PAGES

Blaschke, Daniel N.

2017-10-13

Many materials of interest are polycrystals, i.e., aggregates of single crystals. Randomly distributed orientations of single crystals lead to macroscopically isotropic properties. Here in this paper, we briefly review strategies of calculating effective isotropic second and third order elastic constants from the single crystal ones. Our main emphasis is on single crystals of cubic symmetry. Specifically, the averaging of third order elastic constants has not been particularly successful in the past, and discrepancies have often been attributed to texturing of polycrystals as well as to uncertainties in the measurement of elastic constants of both poly and single crystals. While thismore » may well be true, we also point out here shortcomings in the theoretical averaging framework.« less

Development of a Single-Crystal Fifth-Generation Nickel Superalloy

NASA Astrophysics Data System (ADS)

Petrushin, N. V.; Elyutin, E. S.; Visik, E. M.; Golynets, S. A.

2017-11-01

The chemical and phase compositions of a rhenium-ruthenium-containing fifth-generation VZhM8 nickel superalloy, which is intended for single-crystal turbine blades of an aviation engine, are calculated using computer simulation. VZhM8 alloy <001>, <011>, and <111> single crystals are fabricated. The microstructure, the γ/γ' misfit, the segregation coefficients of alloying elements, the dissolution temperature of the γ' phase, and the solidus and liquidus temperatures of the VZhM8 alloy single crystals in the as-cast state and after heat treatment are studied. The temperature-time dependences of the static elastic modulus, the short-term mechanical properties, and the long-term strength of the alloy single crystals are determined

Effects of heavy-ion irradiation on the microwave surface impedance of (Ba1-x K x )Fe2As2 single crystals

NASA Astrophysics Data System (ADS)

Ghigo, G.; Torsello, D.; Gerbaldo, R.; Gozzelino, L.; Laviano, F.; Tamegai, T.

2018-07-01

The electrodynamic response of Ba1-x K x Fe2As2 single crystals at the microwave frequencies has been investigated by means of a coplanar resonator technique, at different values of non-magnetic disorder introduced into the samples by heavy-ion irradiation. The surface impedance Z s = R s + iX s conforms to the classical skin effect above the critical temperature. Below T c, R s monotonically decreases while X s shows a peak, which evolves as a function of the irradiation fluence. The disorder-dependent Z s (T) curves are analyzed within a two-fluid model, suitably modified to account for a finite quasiparticle fraction at T = 0. The analysis gives, for the unirradiated crystal, quasiparticle relaxation times τ that are in good agreement with previous literature. Smaller τ values are deduced for the disordered crystals, both in the normal and in the superconducting states. The limits of application of the model are discussed.

Suppressing molecular vibrations in organic semiconductors by inducing strain

PubMed Central

Kubo, Takayoshi; Häusermann, Roger; Tsurumi, Junto; Soeda, Junshi; Okada, Yugo; Yamashita, Yu; Akamatsu, Norihisa; Shishido, Atsushi; Mitsui, Chikahiko; Okamoto, Toshihiro; Yanagisawa, Susumu; Matsui, Hiroyuki; Takeya, Jun

2016-01-01

Organic molecular semiconductors are solution processable, enabling the growth of large-area single-crystal semiconductors. Improving the performance of organic semiconductor devices by increasing the charge mobility is an ongoing quest, which calls for novel molecular and material design, and improved processing conditions. Here we show a method to increase the charge mobility in organic single-crystal field-effect transistors, by taking advantage of the inherent softness of organic semiconductors. We compress the crystal lattice uniaxially by bending the flexible devices, leading to an improved charge transport. The mobility increases from 9.7 to 16.5 cm2 V−1 s−1 by 70% under 3% strain. In-depth analysis indicates that compressing the crystal structure directly restricts the vibration of the molecules, thus suppresses dynamic disorder, a unique mechanism in organic semiconductors. Since strain can be easily induced during the fabrication process, we expect our method to be exploited to build high-performance organic devices. PMID:27040501

Suppressing molecular vibrations in organic semiconductors by inducing strain.

PubMed

Kubo, Takayoshi; Häusermann, Roger; Tsurumi, Junto; Soeda, Junshi; Okada, Yugo; Yamashita, Yu; Akamatsu, Norihisa; Shishido, Atsushi; Mitsui, Chikahiko; Okamoto, Toshihiro; Yanagisawa, Susumu; Matsui, Hiroyuki; Takeya, Jun

2016-04-04

Organic molecular semiconductors are solution processable, enabling the growth of large-area single-crystal semiconductors. Improving the performance of organic semiconductor devices by increasing the charge mobility is an ongoing quest, which calls for novel molecular and material design, and improved processing conditions. Here we show a method to increase the charge mobility in organic single-crystal field-effect transistors, by taking advantage of the inherent softness of organic semiconductors. We compress the crystal lattice uniaxially by bending the flexible devices, leading to an improved charge transport. The mobility increases from 9.7 to 16.5 cm(2) V(-1) s(-1) by 70% under 3% strain. In-depth analysis indicates that compressing the crystal structure directly restricts the vibration of the molecules, thus suppresses dynamic disorder, a unique mechanism in organic semiconductors. Since strain can be easily induced during the fabrication process, we expect our method to be exploited to build high-performance organic devices.

Computational modelling of mesoscale dislocation patterning and plastic deformation of single crystals

NASA Astrophysics Data System (ADS)

Xia, Shengxu; El-Azab, Anter

2015-07-01

We present a continuum dislocation dynamics model that predicts the formation of dislocation cell structure in single crystals at low strains. The model features a set of kinetic equations of the curl type that govern the space and time evolution of the dislocation density in the crystal. These kinetic equations are coupled to stress equilibrium and deformation kinematics using the eigenstrain approach. A custom finite element method has been developed to solve the coupled system of equations of dislocation kinetics and crystal mechanics. The results show that, in general, dislocations self-organize in patterns under their mutual interactions. However, the famous dislocation cell structure has been found to form only when cross slip is implemented in the model. Cross slip is also found to lower the yield point, increase the hardening rate, and sustain an increase in the dislocation density over the hardening regime. Analysis of the cell structure evolution reveals that the average cell size decreases with the applied stress, which is consistent with the similitude principle.

Reliability Studies of Ceramic Capacitors.

DTIC Science & Technology

1983-07-01

increases. This case has been found to be a good approximation for single crystals with high chemical and structural purity. Shallow traps may arise as a...theory, this sudden increase may be otherwise explained. Single crystals of ZnS have been found to exhibit this vertical increase in the current...Smith and Rose observed SCLC behavior in CdS single crystals . Branwood and Tredgold 2 8 and Branwood et al. 2 9 measured BaTiO 3 single crystals and

Reversible conversion of valence-tautomeric copper metal-organic frameworks dependent single-crystal-to-single-crystal oxidation/reduction: a redox-switchable catalyst for C-H bonds activation reaction.

PubMed

Huang, Chao; Wu, Jie; Song, Chuanjun; Ding, Ran; Qiao, Yan; Hou, Hongwei; Chang, Junbiao; Fan, Yaoting

2015-06-28

Upon single-crystal-to-single-crystal (SCSC) oxidation/reduction, reversible structural transformations take place between the anionic porous zeolite-like Cu(I) framework and a topologically equivalent neutral Cu(I)Cu(II) mixed-valent framework. The unique conversion behavior of the Cu(I) framework endowed it as a redox-switchable catalyst for the direct arylation of heterocycle C-H bonds.

Solution-grown organic single-crystalline p-n junctions with ambipolar charge transport.

PubMed

Fan, Congcheng; Zoombelt, Arjan P; Jiang, Hao; Fu, Weifei; Wu, Jiake; Yuan, Wentao; Wang, Yong; Li, Hanying; Chen, Hongzheng; Bao, Zhenan

2013-10-25

Organic single-crystalline p-n junctions are grown from mixed solutions. First, C60 crystals (n-type) form and, subsequently, C8-BTBT crystals (p-type) nucleate heterogeneously on the C60 crystals. Both crystals continue to grow simultaneously into single-crystalline p-n junctions that exhibit ambipolar charge transport characteristics. This work provides a platform to study organic single-crystalline p-n junctions. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterization of Molten CZT Using Thermal Conductivity and Heat Capacity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nero, Franco; Jackson, Maxx; Stowe, Ashley

To compare thermal conductivity of a polycrystalline semiconductor to the single crystal semiconductor using thermo-physical data acquired from Simultaneous Thermal Analysis and Transient Plane Source heating.

Growth and nonlinear optical characterization of organic single crystal films

NASA Astrophysics Data System (ADS)

Zhou, Ligui

1997-12-01

Organic single crystal films are important for various future applications in photonics and integrated optics. The conventional method for inorganic crystal growth is not suitable for organic materials, and the high temperature melting method is not good for most organic materials due to decomposition problems. We developed a new method-modified shear method-to grow large area organic single crystal thin films which have exceptional nonlinear optical properties and high quality surfaces. Several organic materials (NPP, PNP and DAST) were synthesized and purified before the thin film crystal growth. Organic single crystal thin films were grown from saturated organic solutions using modified shear method. The area of single crystal films were about 1.5 cm2 for PNP, 1 cm2 for NPP and 5 mm2 for DAST. The thickness of the thin films which could be controlled by the applied pressure ranged from 1μm to 10 μm. The single crystal thin films of organic materials were characterized by polarized microscopy, x-ray diffraction, polarized UV-Visible and polarized micro-FTIR spectroscopy. Polarized microscopy showed uniform birefringence and complete extinction with the rotation of the single crystal thin films under crossed- polarization, which indicated high quality single crystals with no scattering. The surface orientation of single crystal thin films was characterized by x-ray diffraction. The molecular orientation within the crystal was further studied by the polarized UV-Visible and Polarized micro-FTIR techniques combined with the x-ray and polarized microscopy results. A Nd:YAG laser with 35 picosecond pulses at 1064nm wavelength was employed to perform the nonlinear optical characterization of the organic single crystal thin films. Two measurement techniques were used to study the crystal films: second harmonic generation (SHG) and electro-optic (EO) effect. SHG results showed that the nonlinear optical coefficient of NPP was 18 times that of LiNbO3, a standard inorganic crystal material, and the nonlinear optical coefficient of PNP was 11 times that of LiNbO3. Electro-optic measurements showed that r11 = 65 pm/V for NPP and r12 = 350 pm/V for DAST. EO modulation effect was also observed using Fabry-Perot interferometry. Waveguide devices are very important for integrated optics. But the fabrication of waveguide devices on the organic single crystal thin films was difficult due to the solubility of the film in common organic solvents. A modified photolithographic technique was employed to make channel waveguides and poly(vinyl alcohol) (PVA) was used as a protective layer in the fabrication of the waveguides. Waveguides with dimensions about 7/mum x 1μm x 1mm were obtained.

Structure and Growth Control of Organic-Inorganic Halide Perovskites for Optoelectronics: From Polycrystalline Films to Single Crystals.

PubMed

Chen, Yani; He, Minhong; Peng, Jiajun; Sun, Yong; Liang, Ziqi

2016-04-01

Recently, organic-inorganic halide perovskites have sparked tremendous research interest because of their ground-breaking photovoltaic performance. The crystallization process and crystal shape of perovskites have striking impacts on their optoelectronic properties. Polycrystalline films and single crystals are two main forms of perovskites. Currently, perovskite thin films have been under intensive investigation while studies of perovskite single crystals are just in their infancy. This review article is concentrated upon the control of perovskite structures and growth, which are intimately correlated for improvements of not only solar cells but also light-emitting diodes, lasers, and photodetectors. We begin with the survey of the film formation process of perovskites including deposition methods and morphological optimization avenues. Strategies such as the use of additives, thermal annealing, solvent annealing, atmospheric control, and solvent engineering have been successfully employed to yield high-quality perovskite films. Next, we turn to summarize the shape evolution of perovskites single crystals from three-dimensional large sized single crystals, two-dimensional nanoplates, one-dimensional nanowires, to zero-dimensional quantum dots. Siginificant functions of perovskites single crystals are highlighted, which benefit fundamental studies of intrinsic photophysics. Then, the growth mechanisms of the previously mentioned perovskite crystals are unveiled. Lastly, perspectives for structure and growth control of perovskites are outlined towards high-performance (opto)electronic devices.

Ames Lab 101: Single Crystal Growth

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schlagel, Deborah

2013-09-27

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

Ames Lab 101: Single Crystal Growth

ScienceCinema

Schlagel, Deborah

2018-01-16

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

Elastic response of zone axis (001)-oriented PWA 1480 single crystal: The influence of secondary orientation

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

1991-01-01

The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.