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

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.

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.

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.

Single crystalline Co3O4 nanocrystals exposed with different crystal planes for Li-O2 batteries.

PubMed

Su, Dawei; Dou, Shixue; Wang, Guoxiu

2014-08-29

Single crystalline Co3O4 nanocrystals exposed with different crystal planes were synthesised, including cubic Co3O4 nanocrystals enclosed by {100} crystal planes, pseudo octahedral Co3O4 enclosed by {100} and {110} crystal planes, Co3O4 nanosheets exposed by {110} crystal planes, hexagonal Co3O4 nanoplatelets exposed with {111} crystal planes, and Co3O4 nanolaminar exposed with {112} crystal planes. Well single crystalline features of these Co3O4 nanocrystals were confirmed by FESEM and HRTEM analyses. The electrochemical performance for Li-O2 batteries shows that Co3O4 nanocrystals can significantly reduce the discharge-charge over-potential via the effect on the oxygen evolution reaction (OER). From the comparison on their catalytic performances, we found that the essential factor to promote the oxygen evolution reactions is the surface crystal planes of Co3O4 nanocrystals, namely, crystal planes-dependent process. The correlation between different Co3O4 crystal planes and their effect on reducing charge-discharge over-potential was established: {100} < {110} < {112} < {111}.

Synthesis, growth, structural, spectroscopic and optical studies of a new semiorganic nonlinear optical crystal: L-valine hydrochloride.

PubMed

Kirubavathi, K; Selvaraju, K; Valluvan, R; Vijayan, N; Kumararaman, S

2008-04-01

Single crystals of a new semiorganic nonlinear optical (NLO) material, L-valine hydrochloride (LVHCl), having dimensions up to 20 mm x 6 mm x 4 mm have been grown by slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to the monoclinic system. The functional groups presented in the crystal were confirmed by Fourier transform infrared (FTIR) technique. Optical transmission spectrum shows very low absorption in the entire visible region. Differential thermal and thermogravimetric analyses confirmed that the crystal is stable up to 211 degrees C. The powder second harmonic generation (SHG) efficiency of LVHCl is 1.7 times efficient as potassium dihydrogen phosphate (KDP).

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.

Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

NASA Astrophysics Data System (ADS)

Karthigha, S.; Krishnamoorthi, C.

2018-03-01

An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

Effect of the purity of starting materials on the growth and properties of potassium dihydrogen phosphate single crystals – A comparative study

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

Rajesh, P., E-mail: rajeshp@ssn.edu.in; Charoen In, Urit; Manyum, Prapun

2014-11-15

Highlights: • Bulk size KDP crystal has been grown with higher growth rate. • Systematic study on the effect of starting materials has been done. • Crystalline perfection is maintained in the entire crystal. - Abstract: A systematic study on the effect of purity of starting materials on the growth and properties of potassium dihydrogen phosphate single crystals is crucial for the future study of the material for nonlinear optical applications. Potassium dihydrogen phosphate crystals were grown using high pure (99.999%) and ordinary (99.9%) starting raw materials using slow cooling method in identical conditions. Their optical transparency and crystalline perfectionmore » are studied by UV and high resolution X-ray diffraction analyses respectively. The results are checked with the help of etching analyses. The full width at half maximum is 8″ which is close to that expected from the plane wave theory of dynamical X-ray diffraction for an ideally perfect crystal. Results of those studies are correlated with each other. The quantitative results show that the raw material plays an important role in the growth of good quality crystals.« less

Modelling of thermal field and point defect dynamics during silicon single crystal growth using CZ technique

NASA Astrophysics Data System (ADS)

Sabanskis, A.; Virbulis, J.

2018-05-01

Mathematical modelling is employed to numerically analyse the dynamics of the Czochralski (CZ) silicon single crystal growth. The model is axisymmetric, its thermal part describes heat transfer by conduction and thermal radiation, and allows to predict the time-dependent shape of the crystal-melt interface. Besides the thermal field, the point defect dynamics is modelled using the finite element method. The considered process consists of cone growth and cylindrical phases, including a short period of a reduced crystal pull rate, and a power jump to avoid large diameter changes. The influence of the thermal stresses on the point defects is also investigated.

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.

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.

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.

Single Crystalline Co3O4 Nanocrystals Exposed with Different Crystal Planes for Li-O2 Batteries

PubMed Central

Su, Dawei; Dou, Shixue; Wang, Guoxiu

2014-01-01

Single crystalline Co3O4 nanocrystals exposed with different crystal planes were synthesised, including cubic Co3O4 nanocrystals enclosed by {100} crystal planes, pseudo octahedral Co3O4 enclosed by {100} and {110} crystal planes, Co3O4 nanosheets exposed by {110} crystal planes, hexagonal Co3O4 nanoplatelets exposed with {111} crystal planes, and Co3O4 nanolaminar exposed with {112} crystal planes. Well single crystalline features of these Co3O4 nanocrystals were confirmed by FESEM and HRTEM analyses. The electrochemical performance for Li-O2 batteries shows that Co3O4 nanocrystals can significantly reduce the discharge-charge over-potential via the effect on the oxygen evolution reaction (OER). From the comparison on their catalytic performances, we found that the essential factor to promote the oxygen evolution reactions is the surface crystal planes of Co3O4 nanocrystals, namely, crystal planes-dependent process. The correlation between different Co3O4 crystal planes and their effect on reducing charge-discharge over-potential was established: {100} < {110} < {112} < {111}. PMID:25169737

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.

Growth, structural, spectral, optical, and thermal studies on amino acid based new NLO single crystal: L-phenylalanine-4-nitrophenol.

PubMed

Prakash, M; Lydia Caroline, M; Geetha, D

2013-05-01

A new organic nonlinear optical single crystal, L-phenylalanine-4-nitrophenol (LPAPN) belonging to the amino acid group has been successfully grown by slow evaporation technique. The lattice parameters of the grown crystal have been determined by X-ray diffraction studies. FT-IR spectrum was recorded to identify the presence of functional group and molecular structure was confirmed by NMR spectrum. Thermal strength of the grown crystal has been studied using TG-DTA analyses. The grown crystals were found to be transparent in the entire visible region. The existence of second harmonic generation signals was observed using Nd:YAG laser with fundamental wavelength of 1064 nm. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Growth and characterization of Bis(L-threonine) copper (II) monohydrate single crystals: A semiorganic second order nonlinear optical material

NASA Astrophysics Data System (ADS)

Subhashini, R.; Sathya, D.; Sivashankar, V.; Latha Mageshwari, P. S.; Arjunan, S.

2016-12-01

Highly transparent solitary nonlinear semiorganic optical material Bis(L-threonine) copper (II) monohydrate [BLTCM], was synthesized by a conventional slow evaporation solution growth technique. The grown crystals were subjected to structural, optical, electrical, thermal, mechanical, SHG and Laser damage threshold studies. Single crystal XRD shows that the material crystallizes in monoclinic system with noncentrosymmetric space group P21. FT-IR and FT-RAMAN analyses confirm the various functional groups present in the grown crystal. The transparency range of BLTCM was determined by UV-vis-NIR studies and various optical constants such as extinction coefficient (K), refractive index, optical conductivity and electric susceptibility with real and imaginary parts of dielectric constant were calculated using the transmittance data which have applications in optoelectronic devices. Dielectric studies of the crystal were carried out at different frequencies and temperatures to analyze the electrical properties. TGA and DSC analyses were performed to study the thermal behaviour of the sample. The hardness stability of the grown specimen was investigated by Vickers microhardness test. The output intensity of second harmonic generation was confirmed using the Kurtz and Perry powder method. The laser induced surface damage threshold of the crystal was measured using Nd:YAG laser.

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.

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.

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.

The influence of primary and secondary orientations on the elastic response of a nickel-base single-crystal superalloy

NASA Technical Reports Server (NTRS)

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

1993-01-01

The influence of primary orientation on the elastic response of a (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical, thermal, and combined thermal and mechanical loading conditions using finite element techniques. Elastic stress analyses were performed using the MARC finite element code on a square plate of PWA 1480 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 plate were determined for each loading condition. In this paper, the influence of the angular offset between the primary crystal orientation and the loading direction on the elastic stress response of the PWA 1480 plate is presented for different loading conditions. The influence of primary orientation angle, when constrained between the bounds considered, was not found to be as significant as the influence of the secondary orientation angle, which is not typically controlled.

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.

Flexible Semitransparent Energy Harvester with High Pressure Sensitivity and Power Density Based on Laterally Aligned PZT Single-Crystal Nanowires.

PubMed

Zhao, Quan-Liang; He, Guang-Ping; Di, Jie-Jian; Song, Wei-Li; Hou, Zhi-Ling; Tan, Pei-Pei; Wang, Da-Wei; Cao, Mao-Sheng

2017-07-26

A flexible semitransparent energy harvester is assembled based on laterally aligned Pb(Zr 0.52 Ti 0.48 )O 3 (PZT) single-crystal nanowires (NWs). Such a harvester presents the highest open-circuit voltage and a stable area power density of up to 10 V and 0.27 μW/cm 2 , respectively. A high pressure sensitivity of 0.14 V/kPa is obtained in the dynamic pressure sensing, much larger than the values reported in other energy harvesters based on piezoelectric single-crystal NWs. Furthermore, theoretical and finite element analyses also confirm that the piezoelectric voltage constant g 33 of PZT NWs is competitive to the lead-based bulk single crystals and ceramics, and the enhanced pressure sensitivity and power density are substantially linked to the flexible structure with laterally aligned PZT NWs. The energy harvester in this work holds great potential in flexible and transparent sensing and self-powered systems.

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.

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.

Spin glass in semiconducting KFe 1.05 Ag 0.88 Te 2 single crystals

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

Ryu, Hyejin; Lei, Hechang; Klobes, B.

2015-05-01

We report discovery of KFe 1.05 Ag 0.88 Te 2 single crystals with semiconducting spin glass ground state. Composition and structure analyses suggest nearly stoichiometric I 4 / mmm space group but allow for the existence of vacancies, absent in long-range semiconducting antiferromagnet KFe 0.85 Ag 1.15 Te 2 . The subtle change in stoichometry in Fe-Ag sublattice changes magnetic ground state but not conductivity, giving further insight into the semiconducting gap mechanism.

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.

EPR and magnetization studies on single crystals of a heterometallic (Cu II and Cr III) complex: Zero-field splitting determination

NASA Astrophysics Data System (ADS)

Novosel, Nikolina; Žilić, Dijana; Pajić, Damir; Jurić, Marijana; Perić, Berislav; Zadro, Krešo; Rakvin, Boris; Planinić, Pavica

2008-10-01

Magnetic properties of single crystals of the heterometallic complex [Cu(bpy) 3] 2[Cr(C 2O 4) 3]NO 3·9H 2O (bpy = 2,2'-bipyridine) have been investigated. From the recorded EPR spectra, the spin-Hamiltonian parameters have been determined. The magnetization measurements have shown magnetic anisotropy at low temperatures, which has been analysed as a result of the zero-field splitting of the Cr III ion. By fitting the exactly derived magnetization expression to the measured magnetization data, the axial zero-field splitting parameter, D, has been calculated. Comparing to the EPR measurements, it has been confirmed that D can be determined from the measurements of the macroscopic magnetization on the single crystals.

Effects of protein engineering and rational mutagenesis on crystal lattice of single chain antibody fragments

PubMed Central

Kalyoncu, Sibel; Hyun, Jeongmin; Pai, Jennifer C.; Johnson, Jennifer L.; Entzminger, Kevin; Jain, Avni; Heaner, David P.; Morales, Ivan A.; Truskett, Thomas M.; Maynard, Jennifer A.; Lieberman, Raquel L.

2014-01-01

Protein crystallization is dependent upon, and sensitive to, the intermolecular contacts that assist in ordering proteins into a three dimensional lattice. Here we used protein engineering and mutagenesis to affect the crystallization of single chain antibody fragments (scFvs) that recognize the EE epitope (EYMPME) with high affinity. These hypercrystallizable scFvs are under development to assist difficult proteins, such as membrane proteins, in forming crystals, by acting as crystallization chaperones. Guided by analyses of intermolecular crystal lattice contacts, two second-generation anti-EE scFvs were produced, which bind to proteins with installed EE tags. Surprisingly, although non-complementarity determining region (CDR) lattice residues from the parent scFv framework remained unchanged through the processes of protein engineering and rational design, crystal lattices of the derivative scFvs differ. Comparison of energy calculations and the experimentally-determined lattice interactions for this basis set provides insight into the complexity of the forces driving crystal lattice choice and demonstrates the availability of multiple well-ordered surface features in our scFvs capable of forming versatile crystal contacts. PMID:24615866

Synthesis, crystal structure, and magnetic properties of two-dimensional divalent metal glutarate/dipyridylamine coordination polymers, with a single crystal-to-single crystal transformation in the copper derivative

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

Montney, Matthew R.; Supkowski, Ronald M.; Staples, Richard J.

Hydrothermal reaction of divalent metal chlorides with glutaric acid and 4,4'-dipyridylamine (dpa) has afforded an isostructural family of coordination polymers with formulation [M(glu)(dpa)]{sub n} (M=Co (1), Ni (2), Cu (3); glu=glutarate). Square pyramidal coordination is seen in 1-3, with semi-ligation of a sixth donor to produce a '5+1' extended coordination sphere. Neighboring metal atoms are linked into 1D [M(glu)]{sub n} neutral chains through chelating/monodentate bridging glutarate moieties with a syn-anti binding mode, and semi-chelation of the pendant carboxylate oxygen. These chains further connect into 2D layers through dipodal dpa ligands. Neighboring layers stack into the pseudo 3D crystal structure ofmore » 1-3 through supramolecular hydrogen bonding between dpa amine units and the semi-chelated glutarate oxygen atoms. The variable temperature magnetic behavior of 1-3 was explored and modeled as infinite 1D Heisenberg chains. Notably, complex 3 undergoes a thermally induced single crystal-to-single crystal transformation between centric and acentric space groups, with a conformationally disordered unilayer structure at 293 K and an ordered bilayer structure at 173 K. All materials were further characterized via infrared spectroscopy and elemental and thermogravimetric analyses. - Graphical abstract: The coordination polymers [M(glu)(dpa)]{sub n} (M=Co (1), Ni (2), Cu (3); glu=glutarate, dpa=4,4'-dipyridylamine) exhibit 2D layer structures based on 1D [M(glu)]{sub n} chains linked through dpa tethers. Antiferromagnetic coupling is observed for 2 and 3, while ferromagnetism is predominant in 1. Compound 3 undergoes a thermally induced single crystal-to-single crystal transformation from an acentric to a centrosymmetric space group.« less

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

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.

Growth, density functional theory (DFT) and spectral studies on L-2-aminobutyric acid -biologically active material

NASA Astrophysics Data System (ADS)

Usha, C.; Santhakumari, R.; Meenakshi, R.; Jayasree, R.; Bhuvaneswari, M.

2017-12-01

Single crystal of L-2-aminobutyric acid (ABA) was grown from water by slow evaporation at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction studies. The grown crystal was subjected to FT-IR, FT-Raman, 1H NMR and 13C NMR spectral analyses to confirm the presence of functional group and molecular structure respectively. Thermal properties were investigated by thermogravimetric and differential thermal analyses. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. The electronic charge distribution and reactivity of the molecules within the crystal were studied by HOMO and LUMO analysis and the molecular electrostatic potential (MEP) of the grown crystal was performed using the B3LYP method. The anti-bacterial activities of the crystal were performed by disk diffusion method against the standard bacteria E. coli. The crystal exhibits good anti-bacterial activity. Second harmonic generation efficiency of the powdered ABA crystal was tested using Nd:YAG laser and it is found to be ∼3.3 times that of potassium dihydrogen orthophosphate.

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, 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

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.

Structure flexibility of the Cu2ZnSnS4 absorber in low-cost photovoltaic cells: from the stoichiometric to the copper-poor compounds.

PubMed

Choubrac, L; Lafond, A; Guillot-Deudon, C; Moëlo, Y; Jobic, S

2012-03-19

Here we present for the very first time a single-crystal investigation of the Cu-poor Zn-rich derivative of Cu(2)ZnSnS(4). Nowadays, this composition is considered as the one that delivers the best photovoltaic performances in the specific domain of Cu(2)ZnSnS(4)-based thin-film solar cells. The existence of this nonstoichiometric phase is definitely demonstrated here in an explicit and unequivocal manner on the basis of powder and single-crystal X-ray diffraction analyses coupled with electron microprobe analyses. Crystals are tetragonal, space group I ̅4, Z = 2, with a = 5.43440(15) Å and c = 10.8382(6) Å for Cu(2)ZnSnS(4) and a = 5.43006(5) Å and c = 10.8222(2) Å for Cu(1.71)Zn(1.18)Sn(0.99)S(4). © 2012 American Chemical Society

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.

Structural, mechanical and light yield characterisation of heat treated LYSO:Ce single crystals for medical imaging applications

NASA Astrophysics Data System (ADS)

Mengucci, P.; André, G.; Auffray, E.; Barucca, G.; Cecchi, C.; Chipaux, R.; Cousson, A.; Davì, F.; Di Vara, N.; Rinaldi, D.; Santecchia, E.

2015-06-01

Five single crystals of cerium-doped lutetium yttrium oxyorthosilicate (LYSO:Ce) grown by the Czochralski method were submitted to structural characterisation by X-ray (XRD) and neutron (ND) diffraction, scanning (SEM) and transmission (TEM) electron microscopy and energy dispersive microanalysis (EDS). The Ultimate Tensile Strength (UTS), the Young Modulus (YM) and the Light Yield (LY) of the samples were also measured in order to correlate the mechanical and the optical behaviour of the crystals with the characteristics of their microstructure. Two of the samples analysed were also heat treated at 300 °C for 10 h to evidence possible variations induced by the temperature in the optical and mechanical response of the crystals. Results showed that the mean compositional variations evidenced by the structural analyses do not affect the mechanical and optical behaviour of the samples. On the contrary, the thermal treatment could induce the formation of coherent spherical particles (size 10 to 15 nm), not uniformly distributed inside the sample, that strongly reduce the UTS and YM values, but it does not affect the optical response of the crystal. This latter result was attributed to the low value of the heating temperature (300 °C) that is not sufficiently high to induce annealing of the oxygen vacancies traps that are responsible of the deterioration of the scintillation properties of the LYSO:Ce crystals. This study was carried out in the framework of the Crystal Clear Collaboration (CCC).

Physicochemical and crystal structure analyses of the antidiabetic agent troglitazone.

PubMed

Kobayashi, Katsuhiro; Fukuhara, Hiroshi; Hata, Tadashi; Sekine, Akiko; Uekusa, Hidehiro; Ohashi, Yuji

2003-07-01

The antidiabetic agent troglitazone has two asymmetric carbons located at the chroman ring and the thiazolidine ring and is produced as a mixture of equal amounts of four optical isomers, 2R-5S, 2S-5R, 2R-5R, and 2S-5S. The crystalline powdered drug substance consists of two diastereomer pairs, 2R-5R/2S-5S and 2R-5S/2S-5R. There are many types of crystals obtained from various crystallization conditions. The X-ray structure analysis and the physicochemical analyses of troglitazone were performed. The solvated crystals of the 2R-5R/2S-5S pair were crystallized from several solutions: methanol, ethanol, acetonitrile, and dichloromethane. The ratio of solvent and troglitazone was 1 : 2 (L1/2-form). The monohydrate crystals were obtained from aqueous acetone solution (L1-form). On the other hand, only an anhydrate crystal of the 2R-5S/2S-5R pair was crystallized from various solutions (H0-form). The dihydrous mixed crystal (MA2-form) was obtained from a mixture of the two diastereomer pairs of 2R-5R/2S-5S and 2R-5S/2S-5R in equal amounts by the slow evaporation of aqueous acetone solution. The crystal structure of the MA2-form is similar to the H0-form. When the MA2 crystal was kept under low humidity, it was converted into the dehydrated form (MA0-form) with retention of the single crystal form. The structure of the MA0-form is isomorphous to the H0-form. The MA2-form was converted into the MA0-form and vice versa with retention of the single crystal under low and high humidity, respectively. The crystallization and storage conditions of the drug substances were successfully analyzed.

Magnetization Reversal Process of Single Crystal α-Fe Containing a Nonmagnetic Particle

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

Li, Yi; Xu, Ben; Hu, Shenyang Y.

2015-09-25

The magnetization reversal process and hysteresis loops in a single crystal α-iron with nonmagnetic particles are simulated in this work based on the Landau-Lifshitz–Gilbert equation. The evolutions of the magnetic domain morphology are studied, and our analyses show that the magnetization reversal process is affected by the interaction between the moving domain wall and the existing nonmagnetic particles. This interaction strongly depends on the size of the particles, and it is found that particles with a particular size contribute the most to magnetic hardening.

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.

Crystal growth of carbonate apatite using a CaCO3 flux.

PubMed

Suetsugu, Y; Tanaka, J

1999-09-01

Single crystals of carbonate apatite were grown using a CaCO3 flux under an Ar gas pressure of 55 MPa. The crystals obtained were observed by scanning electron microscopy, optical microscopy and X-ray diffraction. Electron probe microanalyses and thermal analyses were performed. CO3 ions in planar triangle form replaced both OH sites and PO4 tetrahedral sites in the apatite structure: in particular, the OH sites were perfectly substituted by CO3 ions using this method.

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.

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.

Synthesis of In2O3 nanostructures with different morphologies as potential supercapacitor electrode materials

NASA Astrophysics Data System (ADS)

Tuzluca, Fatma Nur; Yesilbag, Yasar Ozkan; Ertugrul, Mehmet

2018-01-01

In this study performed using a chemical vapor deposition (CVD) system, one-dimensional (1-D) single crystal indium oxide (In2O3) nanotowers, nanobouqets, nanocones, and nanowires were investigated as a candidate for a supercapacitor electrode material. These nanostructures were grown via Vapor-Liquid-Solid (VLS) and Vapor-Solid (VS) mechanisms according to temperature differences (1000-600 °C). The morphologies, growth mechanisms and crystal structures of these 1-D single crystal In2O3 nanostructures were defined by Field Emission Scanning Electron Microscopy (FESEM), High Resolution Transmission Electron Microscopy (HR-TEM), X-Ray Diffraction (XRD) and Raman Spectroscopy analyses. The elemental analyses of the nanostructures were carried out by energy dispersive X-Ray Spectroscopy (EDS); they gave photoluminescence (PL) spectra with 3.39, 2.65, and 1.95 eV band gap values, corresponding to 365 nm, 467 nm, and 633 wavelengths, respectively. The electrochemical performances of these 1-D single crystal In2O3 nanostructures in an aqueous electrolyte solution (1 M Na2SO4) were determined by Cyclic Voltammetry (CV), Galvanostatic Charge Discharge (GCD) and Electrochemical Impedance Spectroscopy (EIS) analyses. According to GCD measurements at 0.04 mA cm-2 current density, areal capacitance values were 10.1 mF cm-2 and 6.7 mF cm-2 for nanotowers, 12.5 mF cm-2 for nanobouquets, 4.9 mF cm-2 for nanocones, and 16.6 mF cm-2 for nanowires. The highest areal capacitance value was observed in In2O3 nanowires, which retained 66.8% of their initial areal capacitance after a 10000 charge-discharge cycle, indicating excellent cycle stability.

A Novel Coordination Polymer Based on Trinuclear Cobalt Building Blocks Cluster: Synthesis, Crystal Structure, and Properties

NASA Astrophysics Data System (ADS)

Lu, J. F.; Tang, Z. H.; Shi, J.; Ge, H. G.; Jiang, M.; Song, J.; Jin, L. X.

2017-12-01

The title compound {[Co3(μ3-OH)(μ2-H2O)2(H2O)5(BTC)2] · 6H2O} n (H3BTC is a 1,3,5-benzenetricarboxylic acid) was prepared and characterized by single crystal and powder X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric and elemental analyses. The single crystal X-ray diffraction reveals that the title compound consists of 1D infinite zigzag chains which were constructed by trinuclear cobalt cluster and BTC3- ligand. Neighbouring above-mentioned 1D infinite zigzag chains are further linked by intermolecular hydrogen bonding to form a 3D supermolecular structure. In addition, the luminescent properties of the title compound were investigated.

Sequential Linker Installation: Precise Placement of Functional Groups in Multivariate Metal-Organic Frameworks

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

Yuan, S; Lu, WG; Chen, YP

2015-03-11

A unique strategy, sequential linker installation (SLI), has been developed to construct multivariate MOFs with functional groups precisely positioned. PCN-700, a Zr-MOF with eight-connected Zr6O4(OH)(8)(H2O)(4) clusters, has been judiciously designed; the Zr-6 clusters in this MOF are arranged in such a fashion that, by replacement of terminal OH-/H2O ligands, subsequent insertion of linear dicarboxylate linkers is achieved. We demonstrate that linkers with distinct lengths and functionalities can be sequentially installed into PCN-700. Single-crystal to single-crystal transformation is realized so that the positions of the subsequently installed linkers are pinpointed via single-crystal X-ray diffraction analyses. This methodology provides a powerful toolmore » to construct multivariate MOFs with precisely positioned functionalities in the desired proximity, which would otherwise be difficult to achieve.« less

Measurement of ultrashort laser pulses using single-crystal films of 4-aminobenzophenone

NASA Astrophysics Data System (ADS)

Bhowmik, Achintya K.; Tan, Shida; Ahyi, Ayayi C.; Dharmadhikari, J. A.; Dharmadhikari, A. K.; Mathur, D.

2007-12-01

Single-crystal thin-film of an organic second-order nonlinear optical material, 4-aminobenzophenone (ABP), is used to measure the pulsewidth of a Ti-Sapphire laser producing ˜45 fs pulses at 1 kHz repetition rate, by the non-collinear second-harmonic generation (SHG) intensity autocorrelation technique. These films are suitable for measurements over a broad wavelength range, down to 780 nm, due to their wide optical transparency. The single-crystal film with thickness (˜3 μm) less than the coherence length requires no phase-matching for efficient broadband SHG. Pulse walk-off due to group-velocity mismatch (GVM) and temporal broadening of the pulses due to group-velocity dispersion (GVD) are found to be negligible. These effects have been estimated for pulse width down to few-cycle pulses (˜10 fs), and the analyses show that these films can be used to characterize such ultrashort optical pulses.

Growth, spectral, thermal, laser damage threshold, microhardness, dielectric, linear and nonlinear optical properties of an organic single crystal: L-phenylalanine DL-mandelic acid

NASA Astrophysics Data System (ADS)

Jayaprakash, P.; Peer Mohamed, M.; Krishnan, P.; Nageshwari, M.; Mani, G.; Lydia Caroline, M.

2016-12-01

Single crystals of L-phenylalanine dl-mandelic acid [C9H11NO2. C8H8O3], have been grown by the slow evaporation technique at room temperature using aqueous solution. The single crystal XRD study confirms monoclinic system for the grown crystal. The functional groups present in the grown crystal have been identified by FTIR and FT-Raman analyses. The optical absorption studies show that the crystal is transparent in the visible region with a lower cut-off wavelength of 257 nm and the optical band gap energy Eg is determined to be 4.62 eV. The Kurtz powder second harmonic generation was confirmed using Nd:YAG laser with fundamental wavelength of 1064 nm. Further, the thermal studies confirmed no weight loss up to 150°C for the as-grown crystal. The photoluminescence spectrum exhibited three peaks (414 nm, 519 nm, 568 nm) due to the donation of protons from carboxylic acid to amino group. Laser damage threshold value was found to be 4.98 GW/cm2. The Vickers microhardness test was carried out on the grown crystals and there by Vickers hardness number (Hv), work hardening coefficient (n), yield strength (σy), stiffness constant C11 were evaluated. The dielectric behavior of the crystal has been determined in the frequency range 50 Hz-5 MHz at various temperatures.

Does the thermal evolution of molecular structures critically affect the magnetic anisotropy?† †Electronic supplementary information (ESI) available. CCDC 1045631–1045633. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c5sc01245g

PubMed Central

Qian, Kang; Baldoví, José J.; Zhang, Yi-Quan; Overgaard, Jacob; Wang, Bing-Wu

2015-01-01

A dysprosium based single-ion magnet is synthesized and characterized by the angular dependence of the single-crystal magnetic susceptibility. Ab initio and effective electrostatic analyses are performed using the molecular structures determined from single crystal X-ray diffraction at 20 K, 100 K and 300 K. Contrary to the common assumption, the results reveal that the structural thermal effects that may affect the energy level scheme and magnetic anisotropy below 100 K are negligible. PMID:29568416

Single crystal plastic behavior of a single-phase, face-center-cubic-structured, equiatomic FeNiCrCo alloy

DOE PAGES

Wu, Zhenggang; Gao, Y. F.; Bei, Hongbin

2015-07-25

To understand the fundamental deformation mechanisms of compositionally complex alloys, single crystals of a multi-component equiatomic FeNiCoCr alloy with face-centered cubic (FCC) structure were grown for mechanical studies. Similarly to typical FCC pure metals, slip trace analyses indicate that dislocation slips take place on (1 1 1) planes along [11¯0] directions. The critical resolved shear stress (CRSS) obeys the Schmid law at both 77 and 293 K, and tension–compression asymmetry is not observed. Although this material slips in a normal FCC manner both at 293 and 77 K, compared to typical FCC metals the CRSS’s strong temperature dependence is abnormal.

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.

Synthesis, structural, optical, thermal and dielectric studies on new organic nonlinear optical crystal by solution growth technique.

PubMed

Prakash, M; Geetha, D; Lydia Caroline, M

2013-04-15

Single crystals of L-phenylalanine-benzoic acid (LPBA) were successfully grown from aqueous solution by solvent evaporation technique. Purity of the crystals was increased by the method of recrystallization. The XRD analysis confirms that the crystal belongs to the monoclinic system with noncentrosymmetric space group P21. The chemical structure of compound was established by FT-NMR technique. The presence of functional groups was estimated qualitatively by Fourier transform infrared analysis (FT-IR). Ultraviolet-visible spectral analyses showed that the crystal has low UV cut-off at 254 nm combined with very good transparency of 90% in a wide range. The optical band gap was estimated to be 6.91 eV. Thermal behavior has been studied with TGA/DTA analyses. The existence of second harmonic generation (SHG) efficiency was found to be 0.56 times the value of KDP. The dielectric behavior of the sample was also studied for the first time. Copyright © 2013 Elsevier B.V. All rights reserved.

Bis (3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol) organic cocrystal: Synthesis and physico-chemical properties

NASA Astrophysics Data System (ADS)

Sudharsana, N.; Krishnakumar, V.; Nagalakshmi, R.

2016-10-01

A 3-methoxy-4-hydroxybenzaldehyde-2,4,6-trinitrophenol (mhba-tnp) cocrystal was grown by the slow evaporation solution growth technique using ethanol as a solvent. As-grown crystals were characterized by single crystal X-ray diffraction (XRD) study and crystallized with a centrosymmetric space group. Optical properties of the grown crystal have been studied by Ultraviolet-Visible (UV-Vis) absorption spectra in the range from 200 to 800nm and the band gap energy of the crystal was obtained as 2.8eV. Fourier transform infrared (FTIR) and micro Raman spectral analyses have been carried out to confirm the functional groups present in the title compound. Differential scanning calorimetry (DSC) and polarized light thermomicroscopy (PLTM) analyses were carried out to find the melting point. In addition, the optimized geometric parameters and the molecular orbitals were calculated using density functional theory (DFT) with the help of the Gaussian 03W software.

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, 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.

Order-disorder phase transitions and their influence on the structure and vibrational properties of new hybrid material: 2-Amino-4-methyl-3-nitropyridinium trifluoroacetate

NASA Astrophysics Data System (ADS)

Lorenc, J.; Bryndal, I.; Syska, W.; Wandas, M.; Marchewka, M.; Pietraszko, A.; Lis, T.; Mączka, M.; Hermanowicz, K.; Hanuza, J.

2010-08-01

New organic-organic salt, 2-amino-4-methyl-3-nitropyridinium trifluoroacetate, has been synthesised and characterised by FT-IR, FT-Raman, DSC and single crystal X-ray crystallography. The 2-amino-4-methyl-3-nitropyridinium trifluoroacetate undergoes a reversible phase transition at ˜162 K. The X-ray structures, vibrational spectra and quantum chemical DFT calculations (B3LYP/6-31G(d,p) approach) have been analysed for high-temperature and low-temperature modifications of the compound, which both crystallize in orthorhombic space group Pbca with two non-equivalent cations and two anions in the asymmetric unit. Their crystal and molecular structures have been compared and the role of the intermolecular interactions in these crystals has been analysed. The mechanisms of the phase transition have been proposed.

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

Syntheses, structures and properties of two new coordination polymers based on D-camphoric acid and 2-phenyl-4,6-diamino-1,3,5-triazine

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

Lun, Huijie; Yang, Jinghe; Jin, Linyu

2015-05-15

By hydrothermal method, two new coordination polymers [Co(ca)(phdat)]{sub n} (1), [Ni(ca)(phdat).0.125H{sub 2}O]{sub n} (2) (H{sub 2}ca=D-camphoric acid, phdat=2-phenyl-4,6-diamino-1,3,5-triazine) have been achieved and structurally characterized by IR, elemental analyses, X-ray single-crystal diffraction and TGA. The X-ray single-crystal diffraction reveals that compounds 1 and 2 are isostructural, both of which exhibit two-dimensional layered network built up from paddle-wheel Co{sub 2}(CO{sub 2}){sub 4}/Ni{sub 2}(CO{sub 2}){sub 4} SBUs by ca{sup 2−} ligand. In the existence of π…π stacking interactions between triazine rings and phenyl rings, the 3D networks are constructed with the hanging phdat filled between the neighboring layers. Furthermore, compounds 1–2 exhibit antiferromagneticmore » behavior and compound 2 displays a good activity for methanol oxidation. - Graphical abstract: Two new coordination compounds 1–2 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses, magnetic and electrochemical measurement. - Highlights: • This paper reports two new coordination polymers based on D-camphoric acid. • Both the compounds feather two-dimensional layered networks built up from paddle-wheel SBUs. • The magnetism and electrochemical property are investigated.« less

Inelastic neutron scattering experiments with the monochromatic imaging mode of the RITA-II spectrometer

NASA Astrophysics Data System (ADS)

Bahl, C. R. H.; Lefmann, K.; Abrahamsen, A. B.; Rønnow, H. M.; Saxild, F.; Jensen, T. B. S.; Udby, L.; Andersen, N. H.; Christensen, N. B.; Jakobsen, H. S.; Larsen, T.; Häfliger, P. S.; Streule, S.; Niedermayer, Ch.

2006-05-01

Recently a monochromatic multiple data taking mode has been demonstrated for diffraction experiments using a RITA type cold neutron spectrometer with a multi-bladed analyser and a position-sensitive detector. Here, we show how this mode can be used in combination with a flexible radial collimator to perform real inelastic neutron scattering experiments. We present the results from inelastic powder, single crystal dispersion and single crystal constant energy mapping experiments. The advantages and complications of performing these experiments are discussed along with a comparison between the imaging mode and the traditional monochromatic focussing mode.

Single crystals of the 96 K superconductor (Hg,Cu)Ba2CuO4+δ: Growth, structure and magnetism

NASA Astrophysics Data System (ADS)

Pelloquin, D.; Hardy, V.; Maignan, A.; Raveau, B.

1997-02-01

Single crystals of the 1201 (n = 1) (Hg,Cu)Ba2CuO4+δ mercury based cuprate have been grown by using a simple process without dry box. The as-synthesized crystals exhibit constant Tc(onset) of 96 K with sharp superconducting transitions. The electron microscopy coupled with EDX analyses evidence a ``1201''-type structure while a mercury deficiency is observed balanced by an excess of copper. The structural refinements based on single-crystal X-ray diffraction data confirm the electron deficiency on the Hg site (0,0,0) and show a splitting of the latter along the c axis correlated to the partial substitution of Cu for Hg. This structural study leads to the following formula Hg0.84Cu0.16Ba2CuO4.19. The magnetic study of a large crystal (1.1 × 0.38 × 0.065 mm3) shows that the (Hg,Cu)-1201 crystals exhibit an irreversibility line higher than that of the 1201 Hg0.8Bi0.2Ba2CuO4+δ crystal (Tc = 75 K). From the reversible magnetization, a λab(0) = 2470 Å value can be extrapolated. Using a 3D-2D decoupling formula, we obtain γ = 29 for the electronic anisotropy of this phase.

Crystal growth, structural, optical, spectral and thermal studies of tris( L-phenylalanine) L-phenylalaninium nitrate: A new organic nonlinear optical material

NASA Astrophysics Data System (ADS)

Prakash, M.; Geetha, D.; Lydia Caroline, M.

2011-10-01

Tris( L-phenylalanine) L-phenylalaninium nitrate, C 9H 12NO 2+·NO 3-·3C 9H 11NO 2 (TPLPN), a new organic nonlinear optical material was grown from aqueous solution by slow evaporation solution growth at room temperature. The grown crystals were subjected to powder X-ray diffraction and single crystal X-ray diffraction studies to confirm the crystalline nature and crystal structure. The modes of vibration of different molecular groups present in TPLPN have been identified by FTIR spectral analysis. The presence of hydrogen and carbon in the grown crystal were confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. The optical transmission spectral study establishes good transmitting ability of the crystal in the entire visible region. The thermogravimetric (TG) and differential thermal analyses (DTA) were carried out to understand the thermal stability of the sample. The nonlinear optical property of the compound observed using Kurtz powder second harmonic generation test assets the suitability of the grown material for the frequency conversion of laser radiation of Nd:YAG.

Nanomedicine photoluminescence crystal-inspired brain sensing approach

NASA Astrophysics Data System (ADS)

Fang, Yan; Wang, Fangzhen; Wu, Rong

2018-02-01

Precision sensing needs to overcome a gap of a single atomic step height standard. In response to the cutting-edge challenge, a heterosingle molecular nanomedicine crystal was developed wherein a nanomedicine crystal height less than 1 nm was designed and selfassembled on a substrate of either a highly ordered and freshly separated graphite or a N-doped silicon with hydrogen bonding by a home-made hybrid system of interacting single bioelectron donor-acceptor and a single biophoton donor-acceptor according to orthogonal mathematical optimization scheme, and an atomic spatial resolution conducting atomic force microscopy (C-AFM) with MHz signal processing by a special transformation of an atomic force microscopy (AFM) and a scanning tunneling microscopy (STM) were employed, wherein a z axis direction UV-VIS laser interferometer and a feedback circuit were used to achieve the minimized uncertainty of a micro-regional structure height and its corresponding local differential conductance quantization (spin state) process was repeatedly measured with a highly time resolution, as well as a pulsed UV-VIS laser micro-photoluminescence (PL) spectrum with a single photon resolution was set up by traceable quantum sensing and metrology relied up a quantum electrical triangle principle. The coupling of a single bioelectron conducting, a single biophoton photoluminescence, a frequency domain temporal spin phase in nanomedicine crystal-inspired sensing methods and sensor technologies were revealed by a combination of C-AFM and PL measurement data-based mathematic analyses1-3, as depicted in Figure 1 and repeated in nanomedicine crystals with a single atomic height. It is concluded that height-current-phase uncertainty correlation pave a way to develop a brain imaging and a single atomic height standard, quantum sensing, national security, worldwide impact1-3 technology and beyond.

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.

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.

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

Li, Na; Mu, Bao; Lv, Lei

Four new polyoxometalate(POM)–templated metal–organic frameworks based on flexible ligands, namely, [Cu{sub 6}(bip){sub 12}(PMo{sup VI}{sub 12}O{sub 40}){sub 2}(PMo{sup V}Mo{sup VI}{sub 11}O{sub 40}O{sub 2})]·8H{sub 2}O(1), [Cu{sup I}{sub 3}Cu{sup II}{sub 3}(bip){sub 12}(PMo{sup VI}{sub 12}O{sub 40}){sub 2}(PMo{sup V}{sub 12}O{sub 34})]·8H{sub 2}O(2), [Ni{sub 6}(bip){sub 12}(PMo{sup VI}{sub 12}O{sub 40})(PMo{sup VI}{sub 11}Mo{sup V}O{sub 40}){sub 2}]Cl·6H{sub 2}O(3), [Co{sup II}{sub 3}Co{sup III}{sub 2}(H{sub 2}bib){sub 2}(Hbib){sub 2}(PW{sub 9}O{sub 34}){sub 2}(H{sub 2}O){sub 6}]·6H{sub 2}O(4) (bip=1,3-bis(imidazolyl)propane, bib=1,4-bis(imidazolyl)butane) have been obtained under hydrothermal condition and characterized by single-crystal X-ray diffraction analyses, elemental analyses, and thermogravimetric (TG) analyses. The studies of single crystal X-ray indicate that compounds 1–3 crystallize in the trigonal space groupmore » P-3, and compound 4 crystallizes in the triclinic space group P-1. Compounds 1 and 3 represent 3D frameworks, and POMs as the guest molecules are incorporated into the cages which are composed of the ligands and metals, while compounds 2 and 4 show 3D frameworks by hydrogen bonds. This compounds provide new examples of host–guest compounds based on flexible bis(imidazole) ligands. In addition, the electrochemical property and the catalytic property of compound 1 have also been investigated. - Graphical abstract: Four inorganic–organic hybrid compounds based polyoxometalates (POMs) and flexible ligands, namely, have been obtained under hydrothermal conditions and characterized by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra, and thermogravimetric (TG) analyses. Compounds 1–3 are new examples of host–guest compounds based on flexible bis(imidazole) ligands and POMs as the guest molecules are incorporated into the cages which are composed of the ligands and metals. - Highlights: • Polyoxometalate–templated metal–organic frameworks have been prepared. • POMs as the guest molecules are incorporated into the cages. • The cages are flexibility based on flexible bis(imidazole) ligands.« less

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.

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.

A top-down approach to crystal engineering of a racemic Δ2-isoxazoline.

PubMed

Lombardo, Giuseppe M; Rescifina, Antonio; Chiacchio, Ugo; Bacchi, Alessia; Punzo, Francesco

2014-02-01

The crystal structure of racemic dimethyl (4RS,5RS)-3-(4-nitrophenyl)-4,5-dihydroisoxazole-4,5-dicarboxylate, C13H12N2O7, has been determined by single-crystal X-ray diffraction. By analysing the degree of growth of the morphologically important crystal faces, a ranking of the most relevant non-covalent interactions determining the crystal structure can be inferred. The morphological information is considered with an approach opposite to the conventional one: instead of searching inside the structure for the potential key interactions and using them to calculate the crystal habit, the observed crystal morphology is used to define the preferential lines of growth of the crystal, and then this information is interpreted by means of density functional theory (DFT) calculations. Comparison with the X-ray structure confirms the validity of the strategy, thus suggesting this top-down approach to be a useful tool for crystal engineering.

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.

Growth and characterization of a third order nonlinear optical single crystal: Ethylenediamine-4-nitrophenolate monohydrate

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

Dhanalakshmi, B.; Ponnusamy, S., E-mail: suruponnus@gmail.com; Muthamizhchelvan, C.

2015-10-15

Highlights: • EDA4NPH crystal possesses negative nonlinear refractive index. • The crystal exhibits high third-order NLO susceptibility. • Wide transparency of the crystal makes it suitable for NLO applications. • Dielectric studies substantiate the suitability for electro-optic applications. • The crystal possesses suitable mechanical strength for device fabrication. - Abstract: Bulk crystals of the charge-transfer complex, ethylenediamine-4-nitrophenolate monohydrate, were grown by slow solvent evaporation method from aqueous solution at room temperature. The X-ray diffraction measurements showed that the crystal belongs to centrosymmetric space group C2/c of monoclinic system. The functional groups in the complex were identified using FTIR, FTRaman andmore » FTNMR analyses. The Z-scan measurements revealed the negative nonlinear refractive index of the crystal. The nonlinear absorption coefficient and third order nonlinear optical susceptibility calculated from the measurements were −3.5823 × 10{sup −3} cm/W and 2.3762 × 10{sup −6} esu respectively. The crystal was shown to be highly transparent above 366 nm by UV–vis spectroscopy and a yellow fluorescence was observed from PL spectrum. The TG–DTA and DSC analyses showed that the crystal is thermally stable up to 117.4 °C. The crystals were characterized by dielectric, etching and microhardness studies.« less

Helium diffusion experiments on synthetic apatite crystals and single-grain fragments: can we retrieve the He diffusion profiles?

NASA Astrophysics Data System (ADS)

Kasanzu, C.; Beucher, R.; Brown, R. W.; Persano, C.; Stuart, F.

2011-12-01

Apatite (U-Th)/he thermochronometry is one of the most widely used methods of quantifying thermal histories of rocks within the vicinity of the surface. Theoretical and practical development carried out during the last decade, among which was the release of affordable LASERs, have led to standard practice of analyzing single grain rather than multigrain aliquots. The standard theoretical basis for interpreting these ages assumes that the technique is used on full grains. However, the natural weak cleavage of apatite leads to fragmentation of these individual prismatic crystals during the rock crushing and mineral separation process. Apatites are most often broken along a weak cleavage perpendicular to the c-axis. It is therefore common practice to analyze fragments of whole grains, not complete crystals. It is also well known that dating often leads to single ages being more dispersed than expected whatever the efforts to avoid perturbations on the He system. Using a theoretical numerical model and considering both axial and radial diffusion, we demonstrate thata largepart (most?) of the dispersion is due to analyses of single apatite fragments. This effect is larger for older grains which have exprienced a slow cooling history and have well rounded diffusive profiles. Ages are a strongfunction of the fragment size (length specifically), we show that ages from apatite fragments with 1 prismatic termination (1T) can be used to retrieve the helium diffusion profile, provided a sufficient number of single fragment analyses are carried out. The shape of the helium diffusion profile provides a strong constraint on the style of the thermal history and so we propose to use single crystal fragment analyses to extract a mean diffusion profile, and deduce the thermal history of the sample. In order to test these ideas, we performed a set of experiments with natural samples and semi-synthetic grains of apatite. Synthetic grains are obtained by drilling cores of various length/width ratios within standard Durango crystals while natural grains are separated from a deep borehole in south-Africa (BK1) and from the Australian craton. Several experiences are presented: 1) (U-Th)/He dating of about 100 1T single-fragment aliquots of different shape ratio from the BK1 borehole; 2) (U-Th)/He dating of 20 2T single-fragment aliquot from an Australian sample previously dated following standard procedure. 3) (U-Th)/He dating of synthetic fragmentsfrom synthetic grains previously degassed by a known percentageusing a thermo-regulated furnace. The results of the experiments lead to important new insight into the natural dispersion of (U-Th)/He single-grain ages. They show that far from being problematic, highly dispersed data may indeed contain first-order information on the thermal history of rocks. We discuss all the details of the standard (U-Th)/He approach such as the effects of temporally variable diffusivity (e.g. radiation damage models), zonation of U and Th and arbitrary grain size variations.

Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C61-butyric acid methyl ester

NASA Astrophysics Data System (ADS)

Lazzerini, Giovanni Mattia; Paternò, Giuseppe Maria; Tregnago, Giulia; Treat, Neil; Stingelin, Natalie; Yacoot, Andrew; Cacialli, Franco

2016-02-01

We report high-resolution, traceable atomic force microscopy measurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crystals' height. The optical interferometer together with the stabilized laser provides traceability (via the laser wavelength) of the vertical measurements made with the atomic force microscope. We find that the crystals can conform to the surface topography, thanks to their height being significantly smaller compared to their lateral dimensions (namely, heights between about 50 nm and 140 nm, for the crystals analysed, vs. several tens of microns lateral dimensions). The vast majority of the crystals are flat, but an isolated, non-flat crystal provides insights into the growth mechanism and allows identification of "molecular terraces" whose height corresponds to one of the lattice constants of the single PCBM crystal (1.4 nm) as measured with X-ray diffraction.

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.

Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C{sub 61}-butyric acid methyl ester

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

Lazzerini, Giovanni Mattia; Yacoot, Andrew; Paternò, Giuseppe Maria

2016-02-01

We report high-resolution, traceable atomic force microscopy measurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crystals' height. The optical interferometer together with the stabilized laser provides traceability (via the laser wavelength) of the vertical measurements made with the atomic force microscope. We find that the crystals can conform to the surfacemore » topography, thanks to their height being significantly smaller compared to their lateral dimensions (namely, heights between about 50 nm and 140 nm, for the crystals analysed, vs. several tens of microns lateral dimensions). The vast majority of the crystals are flat, but an isolated, non-flat crystal provides insights into the growth mechanism and allows identification of “molecular terraces” whose height corresponds to one of the lattice constants of the single PCBM crystal (1.4 nm) as measured with X-ray diffraction.« less

Enhanced Oxidative Bioremediation of cis-Dichloroethene (cis-DCE) and Vinyl Chloride (VC) using Electron Shuttles

DTIC Science & Technology

2010-02-01

Analyses on a single grain of soil or a single crystal of a precipitate were accomplished using an EMP. Not only can analyses be made on particles as small...24Fe+32 (OH)12[ CO3 ] 54.5% Fe, 41.6% O, 2.0% C 6Fe+2 + CO3 -2 + 12H2O → [Fe+24Fe+32 (OH)12][ CO3 ] (s) + 12H+ + 2e- Mixed ferrous/ferric iron...400 mV DCE: 2,000 Sulfate: ញ mg/L VC: 63 µg/L Seneca Army Depot Activity (Ash Landfill site), New York October-06 Single Double- Wide

Crystal growth, spectral, structural and optical studies of π-conjugated stilbazolium crystal: 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate.

PubMed

Krishna Kumar, M; Sudhahar, S; Bhagavannarayana, G; Mohan Kumar, R

2014-05-05

Nonlinear optical (NLO) organic compound, 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate was synthesized by reflux method. The formation of molecular complex was confirmed from (1)H NMR, FT-IR and FT-Raman spectral analyses. The single crystals were grown by slow evaporation solution growth method and the crystal structure and atomic packing of grown crystal was identified. The morphology and growth axis of grown crystal were determined. The crystal perfection was analyzed using high resolution X-ray diffraction study on (001) plane. Thermal stability, decomposition stages and melting point of the grown crystal were analyzed. The optical absorption coefficient (α) and energy band gap (E(g)) of the crystal were determined using UV-visible absorption studies. Second harmonic generation efficiency of the grown crystal was examined by Kurtz powder method with different particle size using 1064 nm laser. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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.

Structural characterization of cevimeline and its trans-impurity by single crystal XRD.

PubMed

Stepanovs, Dmitrijs; Tetere, Zenta; Rāviņa, Irisa; Kumpiņš, Viktors; Zicāne, Daina; Bizdēna, Ērika; Bogans, Jānis; Novosjolova, Irina; Grigaloviča, Agnese; Meri, Remo Merijs; Fotins, Juris; Čerkasovs, Maksims; Mishnev, Anatoly; Turks, Māris

2016-01-25

Cevimeline is muscarinic receptor agonist which increases secretion of exocrine glands. Cevimeline base is a liquid (m.p. 20-25 °C) at ambient conditions, therefore its pharmaceutical formulation as a solid hydrochloride hemihydrate has been developed. The synthesis of cevimeline yields its cis- and trans-isomers and only the cis-isomer is recognized as the API and used in the finished formulation. In this study structural and physicochemical investigations of hydrochloride hemihydrates of cis- and trans-cevimelines have been performed. Single crystal X-ray analyses of both cis- and trans-isomers of cevimeline are reported here for the first time. It was found that the cis-isomer, the API, has less dense crystal packing, lower melting point and higher solubility in comparison to the trans-isomer. Copyright © 2015 Elsevier B.V. All rights reserved.

Non linear optical studies on semiorganic single crystal: L-arginine 4-nitrophenalate 4-nitrophenol dihydrate (LAPP)

NASA Astrophysics Data System (ADS)

Mahadevan, M.; Sankar, P. K.; Vinitha, G.; Arivanandhan, M.; Ramachandran, K.; Anandan, P.

2017-07-01

L-arginine 4-nitrophenalate 4-nitrophenol dihydrate (LAPP) has been synthesized and grown by solution growth at room temperature using deionized water as a solvent. The various functional groups of the sample were identified by Fourier transform infra-red and Fourier transforms - Raman spectroscopic analyses. The Laser damage threshold of LAPP has been studied. Refractive index of LAPP single crystal was measured using Metricon prism coupler Instrument. The etching studies were carried out to study the quality of the grown crystals. The third order nonlinear optical properties of LAPP sample was analyzed by the Z-scan technique using 532 nm diode pumped CW Nd: YAG laser. The LAPP material exhibits negative optical nonlinearity. The results show that LAPP sample has potential applications in nonlinear optics and it can be exploited for optical limiting or switching.

Tuning hardness in calcite by incorporation of amino acids

NASA Astrophysics Data System (ADS)

Kim, Yi-Yeoun; Carloni, Joseph D.; Demarchi, Beatrice; Sparks, David; Reid, David G.; Kunitake, Miki E.; Tang, Chiu C.; Duer, Melinda J.; Freeman, Colin L.; Pokroy, Boaz; Penkman, Kirsty; Harding, John H.; Estroff, Lara A.; Baker, Shefford P.; Meldrum, Fiona C.

2016-08-01

Structural biominerals are inorganic/organic composites that exhibit remarkable mechanical properties. However, the structure-property relationships of even the simplest building unit--mineral single crystals containing embedded macromolecules--remain poorly understood. Here, by means of a model biomineral made from calcite single crystals containing glycine (0-7 mol%) or aspartic acid (0-4 mol%), we elucidate the origin of the superior hardness of biogenic calcite. We analysed lattice distortions in these model crystals by using X-ray diffraction and molecular dynamics simulations, and by means of solid-state nuclear magnetic resonance show that the amino acids are incorporated as individual molecules. We also demonstrate that nanoindentation hardness increased with amino acid content, reaching values equivalent to their biogenic counterparts. A dislocation pinning model reveals that the enhanced hardness is determined by the force required to cut covalent bonds in the molecules.

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.

Ce{sub 11}Ge{sub 3.73(2)}In{sub 6.27}: Solid-state synthesis, crystal structure and site-preference

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

Jeon, Beom-Yong; Nam, Gnu; Lee, Dong Woo

A novel intermetallic compound of Ce{sub 11}Ge{sub 3.73(2)}In{sub 6.27} has been synthesized through the high-temperature solid-state reaction using Nb-ampoules. A batch of well grown block-/short bar-shaped single-crystals has been obtained, and the crystal structure of the title compound has been characterized by single-crystal X-ray diffraction analyses. Ce{sub 11}Ge{sub 3.73(2)}In{sub 6.27} adopts the Ho{sub 11}Ge{sub 10}-type structure belonging to the tetragonal space group I4/mmm (Z=4, Pearson symbol tI84) with nine crystallographically unique atomic positions in the asymmetric unit. The lattice parameters are a=12.0163(1) Å and c=16.5396(2) Å. The overall crystal structure can simply be depicted as an assembly of three differentmore » types of co-facial cationic polyhedra centered by anions, which is further enclosed by the three-dimensional (3-D) cage-like anionic framework. The extra amount of In is observed in one of three isolated anionic sites resulting in introducing the Ge/In-mixed site at the Wyckoff 4e site. This unique site-preference of In substitution for Ge at the 4e site has been enlightened via the atomic size-aspect which was fully supported and rationalized by the site- and bond-energies analyses using tight-binding linear muffin-tin orbital (TB-LMTO) calculations. Energy-dispersive X-ray spectroscopy (EDS), density of states (DOS), crystal orbital Hamilton population (COHP), and electron localization function (ELF) analyses for the title compound are also presented. Magnetic susceptibility measurement proves that an antiferromagnetic ordering of Ce atoms at a low temperature with a paramagnetic Curie temperature of −23.2 K. - Graphical abstract: Reported is experimental and theoretical investigations for Ce{sub 11}Ge{sub 3.73(2)}In{sub 6.27}, which is the first reported example having the extra amounts of In substitution for Ge at one of three “isolated” anionic sites in the Ho{sub 11}Ge{sub 10}-type phase. The observed In site-preference toward the particular anionic site was rationalized via the atomic size-aspect supported by comprehensive analyses for the site-energies including the Wyckoff 4e and 8j sites. - Highlights: • Block or short-bar shaped single-crystals of Ce{sub 11}Ge{sub 3.73(2)}In{sub 6.27} were synthesized. • The first example of having the In/Ge mixture at the “isolated” anionic site. • The site-preference of In was rationalized by the site- and bond-energies.« less

Crystal growth, structural, optical, spectral and thermal studies of tris(L-phenylalanine)L-phenylalaninium nitrate: a new organic nonlinear optical material.

PubMed

Prakash, M; Geetha, D; Lydia Caroline, M

2011-10-15

Tris(L-phenylalanine)L-phenylalaninium nitrate, C(9)H(12)NO(2)(+)·NO(3)(-)·3C(9)H(11)NO(2) (TPLPN), a new organic nonlinear optical material was grown from aqueous solution by slow evaporation solution growth at room temperature. The grown crystals were subjected to powder X-ray diffraction and single crystal X-ray diffraction studies to confirm the crystalline nature and crystal structure. The modes of vibration of different molecular groups present in TPLPN have been identified by FTIR spectral analysis. The presence of hydrogen and carbon in the grown crystal were confirmed by using proton and carbon nuclear magnetic resonance (NMR) spectral analyses. The optical transmission spectral study establishes good transmitting ability of the crystal in the entire visible region. The thermogravimetric (TG) and differential thermal analyses (DTA) were carried out to understand the thermal stability of the sample. The nonlinear optical property of the compound observed using Kurtz powder second harmonic generation test assets the suitability of the grown material for the frequency conversion of laser radiation of Nd:YAG. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

Synthesis, structural, thermal and optical studies of 1-ethyl-2,6-dimethyl-4-hydroxy pyridinium halides.

PubMed

Dhanuskodi, S; Manivannan, S; Kirschbaum, K

2006-05-15

1-Ethyl-2,6-dimethyl-4-hydroxy pyridinium chloride dihydrate and bromide dihydrate salts have been synthesized and their single crystals were grown by the slow evaporation of aqueous solution at 30 degrees C. The grown crystals were characterized by elemental analysis, FT-NMR and FT-IR techniques to confirm the formation of the expected compound. Optical transmittance window in aqueous solution was found to be 275-1100 nm by UV-vis-NIR technique. Thermogravimetric and differential thermal analyses reveal thermal stability and the presence of two water molecules in the crystal lattices. The crystal structure of chloride salt was also determined by X-ray diffraction method.

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.

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.

Study of magnetic field distribution in anisotropic single twin-boundary magnetic shape memory (MSM) element in actuators

NASA Astrophysics Data System (ADS)

Gabdullin, N.; Khan, S. H.

2017-10-01

Magnetic shape memory effect exhibited by certain alloys at room temperature is known for almost 20 years. The most studied MSM alloys are Ni-Mn-Ga alloys which exhibit up to 12% magnetic field-induced strain (change in shape) depending on microstructure. A multibillion cycle operation without malfunction along with their “smart” properties make them very promising for application in electromagnetic (EM) actuators and sensors. However, considerable twinning stress of MSM crystals resulting in magneto-mechanical hysteresis decreases the efficiency and output force of MSM actuators. Whereas twinning stress of conventional MSM crystals has been significantly decreased over the years, novel crystals with Type II twin boundaries (TBs) possess even lower twinning stress. Unfortunately, the microstructure of MSM crystals with very low twinning stress tends to be unstable leading to their rapid crack growth. Whilst this phenomenon has been studied experimentally, the magnetic field distribution in anisotropic single twin-boundary MSM elements has not been considered yet. This paper analyses the magnetic field distribution in two-variant single twin-boundary MSM elements and discusses its effects on magnetic field-induced stress acting on the twin boundary.

Age of the Lava Creek supereruption and magma chamber assembly at Yellowstone based on 40Ar/39Ar and U-Pb dating of sanidine and zircon crystals

NASA Astrophysics Data System (ADS)

Vazquez, J. A.; Matthews, N. E.; Calvert, A. T.

2015-12-01

The last supereruption from the Yellowstone Plateau formed Yellowstone caldera and ejected the >1000 km3 of rhyolite that composes the Lava Creek Tuff (LCT). Tephra from the eruption blanketed much of the western United States, and is a key Quaternary chronostratigraphic marker, in particular for dating deposition of mid-Pleistocene glacial and pluvial deposits in western North America. We performed 40Ar/39Ar dating of single sanidines to delimit eruption age, and ion microprobe U-Pb and trace-element analyses of crystal faces on single zircons to characterize magmatic evolution and date near-eruption crystallization, as well as analyses of crystal interiors to date the interval of zircon crystallization. Sanidines from the two LCT members A and B yield an 40Ar/39Ar isochron date of 631 ± 4 ka (2σ). Crystal faces on zircons from both members yield a weighted mean 206Pb/238U date of 627 ± 6 ka (2σ) and have trace element concentrations that vary with eruptive stratigraphy. Zircon interiors yield a weighted mean 206Pb/238U date of 660 ± 6 ka, and reveal reverse and/or oscillatory zoning of trace element concentrations, with many crystals containing high-U concentrations and dark cathodoluminescence (CL) cores. These crystals with high-U cores are possibly sourced from 'defrosting' of melt-impregnated margins of the growing subvolcanic reservoir. LCT sanidines mirror the variation of zircon composition within the eruptive stratigraphy, with crystals from upper LCT-A and basal LCT-B having bright-CL rims with high Ba concentrations, suggesting late crystallization after addition of less evolved silicic magma. The occurrence of distal LCT in stratigraphic sequences marking the Marine Isotope Stage 16-15 transition supports the apparent eruption age of ca. 631 ka. These results reveal that Lava Creek zircons record episodic heating, renewed crystallization, and an overall up-temperature evolution for Yellowstone's subvolcanic reservoir in the 103-104 year interval before eruption.

A new Keggin-type polyoxometalate catalyst for degradation of aqueous organic contaminants

NASA Astrophysics Data System (ADS)

Olgun, Asim; Çolak, Alper Tolga; Gübbük, İ. Hilal; Şahin, Onur; Kanar, Ebru

2017-04-01

In this study, a new polyoxometalate, K16[Ni(H2O)6]2[BW12O40]4·48H2O (1) was synthesized at room temperature and characterized by X-ray single crystal diffractions, elemental analyses, IR spectra, and thermo gravimetric analyses (TGA). Crystal structure analysis reveals that compound 1 exhibits a supramolecular structure containing one Keggin-type [BW12O40]4 heteropoly anion. The catalytic properties of this molecule for the degradation of Methyl red (MR), Rhodamine B (RhB), Methyl orange (MO) and Congo red (CR) were investigated. The results show that the compound 1 is a promising catalyst candidate for dye degradation.

Extremely small-core photonic crystal fiber fusion splicing with a single-mode fiber

NASA Astrophysics Data System (ADS)

Tiburcio, Bruno D.; Fernandes, Gil M.; Pinto, Armando N.

2013-11-01

We present a low-loss fusion splicing of a non-linear photonic-crystal fiber (NL-PCF) with a single-mode fiber (SMF), helped by an intermediate fiber, using a electric-arc splicer. We also analysed the splice loss between SMF and intermediate fiber, as a function of the electrical discharge duration, to achieve a low-loss transition between SMF and intermediate fiber, through a thermally expanded core splice (TEC). The NL-PCF has a external cladding diameter of 105 μm, a core diameter of 1.7 μm and mode-field diameter (MFD) of 1.5 μm. We also performed mechanical strength tests to verify the robustness of the splice joints obtained.

Series of chiral interpenetrating 3d-4f heterometallic MOFs: Luminescent sensors and magnetic properties

NASA Astrophysics Data System (ADS)

Zhang, Xiaolei; Chen, Chen; Liu, Xiaoli; Gao, Peng; Hu, Ming

2017-09-01

Series of chiral 3d-4f heterometallic MOFs based on a multidentate terpyridyl carboxylic acid ligand have been synthesized under the solvothermal conditions, namely, [LnZnL(CO3)2(H2O)]n (Ln = Eu (1), Gd (2), Dy (3), Ho (4), Er (5), Tm (6), Yb (7), Lu (8)) (HL = 4‧-(4-carboxyphenyl)-2,2‧:6‧,2″-terpyridine). Compounds 1-8 were structurally characterized by the elemental analyses, infrared spectra, and single crystal X-ray diffractions. Compounds 1-8 exhibit the chiral interpenetrating 3D frameworks. Interestingly, 1 can serve as the luminescent sensor to detect nitrobenzene molecules with high sensitivity. The investigations on CD spectra of single crystals clearly assigned the Cotton effect, indicating that there exist two chiral enantiomers of 1-8 in the course of crystallization. The magnetic properties of 2 and 7 were exploited, respectively.

Tuning hardness in calcite by incorporation of amino acids.

PubMed

Kim, Yi-Yeoun; Carloni, Joseph D; Demarchi, Beatrice; Sparks, David; Reid, David G; Kunitake, Miki E; Tang, Chiu C; Duer, Melinda J; Freeman, Colin L; Pokroy, Boaz; Penkman, Kirsty; Harding, John H; Estroff, Lara A; Baker, Shefford P; Meldrum, Fiona C

2016-08-01

Structural biominerals are inorganic/organic composites that exhibit remarkable mechanical properties. However, the structure-property relationships of even the simplest building unit-mineral single crystals containing embedded macromolecules-remain poorly understood. Here, by means of a model biomineral made from calcite single crystals containing glycine (0-7 mol%) or aspartic acid (0-4 mol%), we elucidate the origin of the superior hardness of biogenic calcite. We analysed lattice distortions in these model crystals by using X-ray diffraction and molecular dynamics simulations, and by means of solid-state nuclear magnetic resonance show that the amino acids are incorporated as individual molecules. We also demonstrate that nanoindentation hardness increased with amino acid content, reaching values equivalent to their biogenic counterparts. A dislocation pinning model reveals that the enhanced hardness is determined by the force required to cut covalent bonds in the molecules.

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

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.

Structural, thermal, laser damage, photoconductivity, NLO and mechanical properties of modified vertical Bridgman method grown AgGa0.5In0.5Se2 single crystal

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-08-01

AgGa0.5In0.5Se2 single crystal was grown using modified vertical Bridgman method. The structural perfection of the AgGa0.5In0.5Se2 single crystal has been analyzed by high-resolution X-ray diffraction rocking curve measurements. The structural and compositional uniformities of AgGa0.5In0.5Se2 were studied using Raman scattering spectroscopy at room temperature. The FWHM of the Γ1 (W1) and Γ5L (Γ15) measured at different regions of the crystal confirms that the composition throughout its length is fairly uniform. Thermal properties of the as-grown crystal, including specific heat, thermal diffusivity and thermal conductivity have been investigated. The multiple shot surface laser damage threshold value was measured using Nd:YAG laser. Photoconductivity measurements with different temperatures have confirmed the positive photoconducting behavior. Second harmonic generation (SHG) on powder samples has been measured using the Kurtz and Perry technique and the results display that AgGa0.5In0.5Se2 is a phase-matchable NLO material. The hardness behavior has been measured using Vickers micro hardness measurement and the indentation size effect has been observed. The classical Meyer's law, propositional resistance model and modified propositional resistance model have been used to analyse the micro hardness behavior.

Spatially resolved analysis of short-range structure perturbations in a plastically bent molecular crystal

NASA Astrophysics Data System (ADS)

Panda, Manas K.; Ghosh, Soumyajit; Yasuda, Nobuhiro; Moriwaki, Taro; Mukherjee, Goutam Dev; Reddy, C. Malla; Naumov, Panče

2015-01-01

The exceptional mechanical flexibility observed with certain organic crystals defies the common perception of single crystals as brittle objects. Here, we describe the morphostructural consequences of plastic deformation in crystals of hexachlorobenzene that can be bent mechanically at multiple locations to 360° with retention of macroscopic integrity. This extraordinary plasticity proceeds by segregation of the bent section into flexible layers that slide on top of each other, thereby generating domains with slightly different lattice orientations. Microscopic, spectroscopic and diffraction analyses of the bent crystal showed that the preservation of crystal integrity when stress is applied on the (001) face requires sliding of layers by breaking and re-formation of halogen-halogen interactions. Application of stress on the (100) face, in the direction where π···π interactions dominate the packing, leads to immediate crystal disintegration. Within a broader perspective, this study highlights the yet unrecognized extraordinary malleability of molecular crystals with strongly anisotropic supramolecular interactions.

Synthesis, Structural and Antioxidant Studies of Some Novel N-Ethyl Phthalimide Esters

PubMed Central

Chandraju, Siddegowda; Win, Yip-Foo; Tan, Weng Kang; Quah, Ching Kheng; Fun, Hoong-Kun

2015-01-01

A series of N-ethyl phthalimide esters 4(a-n) were synthesized and characterized by spectroscopic studies. Further, the molecular structure of majority of compounds were analysed by single crystal X-ray diffraction studies. The X-ray analysis revealed the importance of substituents on the crystal stability and molecular packing. All the synthesized compounds were tested for in vitro antioxidant activity by DPPH radical scavenging, FRAP and CUPRAC methods. Few of them have shown good antioxidant activity. PMID:25742494

Synthesis, structural and antioxidant studies of some novel N-ethyl phthalimide esters.

PubMed

Chidan Kumar, C S; Loh, Wan-Sin; Chandraju, Siddegowda; Win, Yip-Foo; Tan, Weng Kang; Quah, Ching Kheng; Fun, Hoong-Kun

2015-01-01

A series of N-ethyl phthalimide esters 4(a-n) were synthesized and characterized by spectroscopic studies. Further, the molecular structure of majority of compounds were analysed by single crystal X-ray diffraction studies. The X-ray analysis revealed the importance of substituents on the crystal stability and molecular packing. All the synthesized compounds were tested for in vitro antioxidant activity by DPPH radical scavenging, FRAP and CUPRAC methods. Few of them have shown good antioxidant activity.

Feasibilty analyses of electroepitaxial research and development accomodations. Volume 1: Accommodations assessment

NASA Technical Reports Server (NTRS)

1983-01-01

A preliminary assessment of the feasibility of accommodating the on-orbit R&D requirements for electroepitaxial crystal growth using the Orbiter middeck, the Materials Experiment Assembly or the Get-Away Special cans was performed. The study is based on the proposed electroepitaxial growth of single crystals of gallium arsenide (GaAs). Baseline R&D requirements, synthesizing furnace and facility conceptual design requirements, accommodation requirements, preliminary compatibility assessments are established. The systems engineering approach employed for the individual assessments is outlined.

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

Luong Thi, T. T., E-mail: thuyltt@hnue.edu.vn; Nguyen Bich, N.; Nguyen, H.

Two 4-substituted 2,2'-bipyridines, namely 4-(ferrocenylethynyl)-2,2'-bipyridine (I) and 4-ferrocenyl-2,2'-bipyridine (II) have been synthesized and fully characterized via single-crystal X-ray diffraction and {sup 1}H and {sup 13}C NMR analyses. The π-conjugated system designed from 2,2'-bipyridine modified with the ferrocenylethynyl and ferrocenyl groups shows the desired planarity. In the crystal packing of I and II, the molecules arrange themselves in head-to-tail and head-to-head motifs, respectively, resulting in consecutive layers of ferrocene and pyridine moieties.

One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

NASA Astrophysics Data System (ADS)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

2016-11-01

Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

Screening and structural elucidation of the zwitterionic cocrystal o-picolinic acid with p-nitro aniline

NASA Astrophysics Data System (ADS)

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

2017-04-01

The cocrystal was screened by solvent drop grinding method and the crystals were grown by slow evaporation method at ambient conditions. The cocrystal formation of o-picolinic acid with p-nitro aniline was initially analysed by powder X-ray diffraction. Further the structural properties of the grown crystal were confirmed by the single X-ray diffraction which indicates that the cocrystal were connected by the strong N+sbnd H-⋯O hydrogen bond interaction. The cell parameters of the grown crystal were a = 14.2144(5) Å, b = 5.7558(2) Å, c = 16.0539(6) Å. The functional groups were identified using Fourier transform infrared and Raman spectral analysis. The excitation and emission state of the sample was analysed by the UV-Visible and Fluorescence studies. The red emission was observed from the Fluorescence studies. NMR studies revealed the chemical shift of the cocrystal. Thermal stability and its melting behaviour were studied by TGA and DSC analytical techniques. Electrical behaviour was studied using the dielectric studies. The intermolecular charge transfer within the molecule were analysed using HOMO- LUMO plots.

Growth and characterization of novel organic 3-Hydroxy Benzaldehyde-N-methyl 4 Stilbazolium Tosylate crystals for NLO applications.

PubMed

Jagannathan, K; Umarani, P; Ratchagar, V; Ramesh, V; Kalainathan, S

2016-01-15

The 3-Hydroxy Benzaldehyde-N-methyl 4-Stilbazolium Tosylate (3- HBST) is a new organic NLO crystal and it is a new derivative in stilbazolium tosylate family. In this work we have synthesized 3-HBST and the single crystal was grown by conventional slow cooling method. The structure and lattice parameters of the grown crystal were determined by the single crystal X-ray diffraction (XRD) technique and it is exhibiting good crystalline nature which is observed from the powder XRD. In order to check the crystalline quality the rocking curve was recorded using multi crystal X-ray diffractometer. The functional groups were identified from both FTIR and NMR spectral analyses. The π-π* and n-π* optical transition energy levels were estimated from the absorption peaks. The NLO property was confirmed by measuring relative SHG efficiency by Kurtz powder test; it shows 24 times higher SHG efficiency than that of urea. In order to test the mechanical stability the Vickers and Knoop micro hardness measurement were carried out and found that the micro hardness number decreases with increasing load. The melting point was determined from Differential Scanning Colorimetry (DSC). Copyright © 2015 Elsevier B.V. All rights reserved.

Phase equilibria in the quasiternary system Ag2S-Ga2S3-In2S3 and optical properties of (Ga55In45)2S300, (Ga54.59In44.66Er0.75)2S300 single crystals

NASA Astrophysics Data System (ADS)

Ivashchenko, I. A.; Danyliuk, I. V.; Olekseyuk, I. D.; Pankevych, V. Z.; Halyan, V. V.

2015-07-01

The quasiternary system Ag2S-Ga2S3-In2S3 was investigated by differential thermal, X-ray diffraction analyses. The phase diagram of the Ga2S3-In2S3 system and nine polythermal sections, isothermal section at 820 K and the liquidus surface projection were constructed. The existence of the large solid solutions ranges of binary and ternary compounds was established. The range of the existence of the quaternary phase AgGaxIn5-xS8 (2.25≤x≤2.85) at 820 K was determined. The single crystals (Ga55In45)2S300 and (Ga54.59In44.66Er0.75)2S300 were grown by a directional crystallization method from solution-melt. Optical absorption spectra in the 500-1600 nm range were recorded. The luminescence of the (Ga54.59In44.66Er0.75)2S300 single crystal shows a maximum at 1530 nm for the excitation wavelengths of 532 and 980 nm at 80 and 300 K.

Design, structural investigation and physicochemical properties of benzotriazolium m-nitrophthalate monohydrate single crystals

NASA Astrophysics Data System (ADS)

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

2018-04-01

The single crystals of organic salt benzotriazolium m-nitrophthalate monohydrate were grown by slow evaporation technique. It crystallizes in orthorhombic system with space group Pbca. The molecular interactions of the compound have been pictured using Hirshfeld surfaces and fingerprints plots and the results were compared with BZD+·mNPA-. The functional groups were identified by FTIR and FT-Raman spectra. The proton transfer from acid to base was identified from the 1H and 13C NMR spectra. The absorption and emission spectrum of BTA+·mNPA-·H2O was recorded in aqueous solution and different solvents, respectively The HOMO and LUMO energy gap of benzotriazole and BTA+·mNPA-·H2O were calculated using density functional theory (DFT). The thermal stability and melting point of hydrated salt was analysed and compared by TG-DTG/DSC study. The anti-oxidant activity of the title compound was evaluated by DPPH and ABTS+ Radical scavenging assay. The anti-microbial and anti-cancer activity showed a potential impact in the crystal.

Heterojunction photodiode on cleaved SiC

NASA Astrophysics Data System (ADS)

Solovan, Mykhailo M.; Farah, John; Kovaliuk, Taras T.; Brus, Viktor V.; Mostovyi, Andrii I.; Maistruk, Eduard V.; Maryanchuk, Pavlo D.

2018-01-01

Graphite/n-SiC Shottky diodes were prepared by means of the recently proposed technique based on the transferring of drawn graphite films onto the n-SiC single crystal substrate. Current-voltage characteristics were measured and analyzed. High quality ohmic contancts were prepared by the DC magnetron sputtering of Ni thin films onto cleaved n-type SiC single crystal substrates. The height of the potential barrier and the series resistance of the graphite/n-SiC junctions were measured and analysed. The dominant current transport mechanisms through the diodes were determined. There was shown that the dominant current transport mechanisms through the graphite/n-SiC Shottky diodes were the multi-step tunnel-recombination at forward bias and the tunnelling mechanisms at reverse bias.

Micromechanics of Sea Urchin spines.

PubMed

Tsafnat, Naomi; Fitz Gerald, John D; Le, Hai N; Stachurski, Zbigniew H

2012-01-01

The endoskeletal structure of the Sea Urchin, Centrostephanus rodgersii, has numerous long spines whose known functions include locomotion, sensing, and protection against predators. These spines have a remarkable internal microstructure and are made of single-crystal calcite. A finite-element model of the spine's unique porous structure, based on micro-computed tomography (microCT) and incorporating anisotropic material properties, was developed to study its response to mechanical loading. Simulations show that high stress concentrations occur at certain points in the spine's architecture; brittle cracking would likely initiate in these regions. These analyses demonstrate that the organization of single-crystal calcite in the unique, intricate morphology of the sea urchin spine results in a strong, stiff and lightweight structure that enhances its strength despite the brittleness of its constituent material.

Crystal structure determination of new antimitotic agent bis(p-fluorobenzyl)trisulfide.

PubMed

An, Haoyun; Hu, Xiurong; Gu, Jianming; Chen, Linshen; Xu, Weiming; Mo, Xiaopeng; Xu, Wanhong; Wang, Xiaobo; Xu, Xiao

2008-01-01

The purpose of this research was to investigate the physical characteristics and crystalline structure of bis(p-fluorobenzyl)trisulfide, a new anti-tumor agent. Methods used included X-ray single crystal diffraction, X-ray powder diffraction (XRPD), Fourier-transform infrared (FT-IR) spectroscopy, differential scanning calorimetric (DSC) and thermogravimetric (TG) analyses. The findings obtained with X-ray single crystal diffraction showed that a monoclinic unit cell was a = 12.266(1) A, b = 4.7757(4) A, c = 25.510(1) A, beta = 104.25(1) degrees ; cell volume = 1,448.4(2) A(3), Z = 4, and space group C2/c. The XRPD studies of the four crystalline samples, obtained by recrystallization from four different solvents, indicated that they had the same diffraction patterns. The diffraction pattern stimulated from the crystal structure data is in excellent agreement with the experimental results. In addition, the identical FT-IR spectra of the four crystalline samples revealed absorption bands corresponding to S-S and C-S stretching as well as the characteristic aromatic substitution. Five percent weight loss at 163.3 degrees C was observed when TG was used to study the decomposition process in the temperature range of 20-200 degrees C. DSC also allowed for the determination of onset temperatures at 60.4(1)-60.7(3) degrees C and peak temperatures at 62.1(3)-62.4(3) degrees C for the four crystalline samples studied. The results verified that the single crystal structure shared the same crystal form with the four crystalline samples investigated.

Astronaut Scott Parazynski works with PCG experiment on middeck

NASA Image and Video Library

1994-11-14

STS066-13-029 (3-14 Nov 1994) --- On the Space Shuttle Atlantis' mid-deck, astronaut Scott E. Parazynski, mission specialist, works at one of two areas onboard the Shuttle which support the Protein Crystal Growth (PCG) experiment. This particular section is called the Vapor Diffusion Apparatus (VDA), housed in a Single Locker Thermal Enclosure (STES). Together with the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES) the VDA represents the continuing research into the structures of proteins and other macromolecules such as viruses. In addition to using the microgravity of space to grow high-quality protein crystals for structural analyses, the experiments are expected to help develop technologies and methods to improve the protein crystallization process on Earth as well as in space.

Crystal structure, thermal and optical properties of Benzimidazole benzimidazolium picrate crystal

NASA Astrophysics Data System (ADS)

Jagadesan, A.; Peramaiyan, G.; Srinivasan, T.; Kumar, R. Mohan; Arjunan, S.

2016-02-01

A new organic framework of benzimidazole with picric acid has been synthesized. A single crystal with a size of 38×10×4 mm3 was grown by a slow evaporation solution growth technique. X-ray diffraction study revealed that the BZP crystal belongs to triclinic system with space group P-1. High resolution X-ray diffraction study shows the absence of grain boundaries without any defects. The thermal stability and specific heat capacity of BZP were investigated by TG/DT and TG/DSC analyses. From the UV-vis-NIR spectral study, optical transmission window and band gap of BZP were found out. The nonlinear refractive index (n2) and third order susceptibility Re(χ(3)) values of BZP crystal are estimated to be 1.73×10-7 cm2/W and 1.26×10-5 esu, respectively using a Z-scan technique.

Ion beam modification of single crystalline BiVO4

NASA Astrophysics Data System (ADS)

Wendler, Elke; Bischoff, Marie; Schmidt, Emanuel; Schrempel, F.; Ellmer, Klaus; Kanis, Michael; van de Krol, Roel

2017-10-01

A single crystalline BiVO4 sample was investigated. Angular resolved Rutherford backscattering spectrometry (arRBS) was performed as a function of two orthogonal angles perpendicular to the surface. The crystal planes appearing in the angular charts are compared with the crystal structure of monoclinic BiVO4. By this comparison the crystal axis being almost normal to the surface was identified to be 〈0 0 1〉. These measurements support the control of orientation and quality of the grown BiVO4 crystal. Additionally it is found that during prolonged analysis the He ions produce a considerable amount of damage. As the nuclear energy loss of the He ions is negligibly low within the corresponding depth region, the damage is mainly caused by the electronic energy loss of the ions. For studying radiation resistance and damage formation, the BiVO4 single crystal was implanted with 200 keV Ar ions. The damage production in the Bi sublattice was analysed by RBS applying 1.8 MeV He ions in channelling configuration. The damage profiles determined from the channelling RBS spectra can be well represented by the electronic energy loss of the implanted Ar ions. From this it is concluded that, in agreement with the finding mentioned above, this energy mainly triggers damage formation in ion irradiated BiVO4. The energy for producing one displaced Bi atom as seen by RBS decreases with increasing damage concentration and varies between 33 and 3.4 eV.

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

Cyanide bridged hetero-metallic polymeric complexes: Syntheses, vibrational spectra, thermal analyses and crystal structures of complexes [M(1,2-dmi)2Ni(μ-CN)4]n (M = Zn(II) and Cd(II))

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Sayın, Elvan; Şahin, Onur

2015-12-01

Two cyanide bridged hetero-metallic complexes of general formula, [M(1,2-dmi)2Ni(μ-CN)4]n (1,2-dmi = 1,2-dimethylimidazole and M = Zn(II) or Cd(II)) have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal analyses and elemental analyses. The crystallographic analyses reveal that the complexes, [Zn(1,2-dmi)2Ni(μ-CN)4] (1) and [Cd(1,2-dmi)2Ni(μ-CN)4] (2), have polymeric 2D networks. In the complexes, four cyanide groups of [Ni(CN)4]2- coordinated to the adjacent M(II) ions and distorted octahedral geometries of complexes are completed by two nitrogen atoms of trans 1,2-dmi ligands. The structures of 1 and 2 are similar and linked via intermolecular hydrogen bonding, C-H⋯Ni interactions to give rise to 3D networks. Vibration assignments are given for all the observed bands and the spectral features also supported to the crystal structures of heteronuclear complexes. The FT-IR and Raman spectra of the complexes are very much consistent with the structural data presented.

Synthesis, nucleation, growth, structural, spectral, thermal, linear and nonlinear optical studies of novel organic NLO crystal: 4-fluoro 4-nitrostilbene (FONS).

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-03-15

A novel organic nonlinear optical material 4-fluoro 4-nitrostilbene (FONS), with molecular formula (C(14)H(10)FNO(2)) has been synthesized. Using ethyl methyl ketone as solvent, the synthesized material has been repeatedly recrystallized to minimize the impurities and good optical quality single crystals were harvested by slow evaporation method. Single crystal X-ray diffraction analysis reveals that the grown FONS crystal belongs to monoclinic system with noncentrosymmetric space group "P2(1)". The powder X-ray diffraction pattern of FONS has been recorded. Functional groups of the title compound were confirmed by FTIR and the molecular structure was confirmed by (1)HNMR. The UV-vis-NIR absorption study reveals no absorption in the visible region and the cut-off wavelength was found to be at 408 nm. Optical band gap (E(g)) of the grown crystal was found to be 3.27 eV and also the optical constants were determined. Thermal behaviour of the FONS has been studied by TGA/DTA analyses. From the mass spectrum, the ratio of compound formation of FONS was analyzed. The NLO property has been confirmed by Kurtz and Perry powder SHG technique and the SHG efficiency of FONS (262 mV) crystal was found to be 12 times greater than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Crystalline inclusions in the cytoplasm and nuclei of cells of acute myeloid leukaemia.

PubMed

Pearson, E C

1989-01-01

In a survey by electron microscopy of peripheral blood and/or bone marrow from 230 adult patients with acute myeloid leukaemia, five were observed to contain crystalline inclusions in the cytoplasm of the leukaemic cells and a sixth contained crystals in the nuclei. In four cases, two of FAB type M2 and two of M4, the cytoplasmic crystals were hexagonal in section and 1-2 micron long. Two examples showed internal periodicities in the range 3.3-4.0 nm when the electronmicrographs were analysed by optical diffractometry. A single case of M1 contained smaller trapezoidal crystals with a 4.9nm periodicity. The sixth patient, with unusual cytological abnormalities and a rare t(3; 6) chromosomal translocation, contained six-sided crystals in the nuclei of some relatively undifferentiated cells. To the best of our knowledge such intranuclear crystals have not previously been reported in leukaemia. The relevance of the crystals to the leukaemic process is discussed.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

2016-10-01

Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

PubMed Central

Nederlof, Igor; van Genderen, Eric; Li, Yao-Wang; Abrahams, Jan Pieter

2013-01-01

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLM and SCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins. PMID:23793148

Crystal growth, differential gas adsorption, high thermal stability, and reversible coordination of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O)

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

Halake, Shobha; Ok, Kang Min, E-mail: kmok@cau.ac.kr

2015-11-15

Single crystals of two barium-organic framework materials, Ba(SBA)(DMF){sub 4} (CAUMOF-15) and Ba{sub 2}(BTEC)(H{sub 2}O) (CAUMOF-16), have been grown through solvothermal reactions (H{sub 2}SBA=4,4′-sulfonyldibenzoic acid and H{sub 4}BTEC=1,2,4,5-benzenetetracarboxylic acid). The crystal structures of the reported frameworks have been determined by single-crystal X-ray diffraction. The materials have been fully characterized by powder X-ray diffraction (PXRD), elemental analyses, Infrared (IR) spectroscopy, and thermogravimetric analyses (TGA). CAUMOF-15 reveals a three-dimensional open-framework that comprises of an inorganic motif with one-dimensional chains and the SBA linkers. CAUMOF-16 shows another three-dimensional backbone consisting of layers of edge-shared BaO{sub 9} and BaO{sub 10} polyhedra, and BTEC pillars. Bothmore » of the 3D frameworks exhibit relatively high thermal stabilities. The PXRD and IR spectral data confirm that CAUMOF-15 and CAUMOF-16 reveal reversible coordinations of the respective solvent molecules, DMF and H{sub 2}O. Gas adsorption properties towards nitrogen, hydrogen, and carbon dioxide have been also investigated. - Graphical abstract: Crystals of two new barium-organic frameworks, Ba(SBA)(DMF){sub 4} and Ba{sub 2}(BTEC)(H{sub 2}O), exhibiting a differential gas adsorption, a high thermal stability, and a reversible coordination of solvent molecules have been grown. - Highlights: • Crystals of two new 3D Ba-MOFs are grown. • The two Ba-MOFs reveal very high thermal stabilities up to ca. 400 °C. • Ba(SBA)(DMF){sub 4} exhibits differential gas adsorption properties. • The two Ba-MOFs show reversible coordination of the solvent molecules.« less

Micromechanics of Sea Urchin Spines

PubMed Central

Tsafnat, Naomi; Fitz Gerald, John D.; Le, Hai N.; Stachurski, Zbigniew H.

2012-01-01

The endoskeletal structure of the Sea Urchin, Centrostephanus rodgersii, has numerous long spines whose known functions include locomotion, sensing, and protection against predators. These spines have a remarkable internal microstructure and are made of single-crystal calcite. A finite-element model of the spine’s unique porous structure, based on micro-computed tomography (microCT) and incorporating anisotropic material properties, was developed to study its response to mechanical loading. Simulations show that high stress concentrations occur at certain points in the spine’s architecture; brittle cracking would likely initiate in these regions. These analyses demonstrate that the organization of single-crystal calcite in the unique, intricate morphology of the sea urchin spine results in a strong, stiff and lightweight structure that enhances its strength despite the brittleness of its constituent material. PMID:22984468

On the colour of wing scales in butterflies: iridescence and preferred orientation of single gyroid photonic crystals

PubMed Central

2017-01-01

Lycaenid butterflies from the genera Callophrys, Cyanophrys and Thecla have evolved remarkable biophotonic gyroid nanostructures within their wing scales that have only recently been replicated by nanoscale additive manufacturing. These nanostructures selectively reflect parts of the visible spectrum to give their characteristic non-iridescent, matte-green appearance, despite a distinct blue–green–yellow iridescence predicted for individual crystals from theory. It has been hypothesized that the organism must achieve its uniform appearance by growing crystals with some restrictions on the possible distribution of orientations, yet preferential orientation observed in Callophrys rubi confirms that this distribution need not be uniform. By analysing scanning electron microscope and optical images of 912 crystals in three wing scales, we find no preference for their rotational alignment in the plane of the scales. However, crystal orientation normal to the scale was highly correlated to their colour at low (conical) angles of view and illumination. This correlation enabled the use of optical images, each containing up to 104–105 crystals, for concluding the preferential alignment seen along the at the level of single scales, appears ubiquitous. By contrast, orientations were found to occur at no greater rate than that expected by chance. Above a critical cone angle, all crystals reflected bright green light indicating the dominant light scattering is due to the predicted band gap along the direction, independent of the domain orientation. Together with the natural variation in scale and wing shapes, we can readily understand the detailed mechanism of uniform colour production and iridescence suppression in these butterflies. It appears that the combination of preferential alignment normal to the wing scale, and uniform distribution within the plane is a near optimal solution for homogenizing the angular distribution of the band gap relative to the wings. Finally, the distributions of orientations, shapes, sizes and degree of order of crystals within single scales provide useful insights for understanding the mechanisms at play in the formation of these biophotonic nanostructures. PMID:28630678

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.

Synthesis and characterization of 3-acetoxy-2-methyl-N-(phenyl)benzamide and 3-acetoxy-2-methyl-N-(4- methylphenyl)benzamide

NASA Astrophysics Data System (ADS)

Kırca, Başak Koşar; Çakmak, Şükriye; Kütük, Halil; Odabaşoğlu, Mustafa; Büyükgüngör, Orhan

2018-01-01

This study treats about two successfully synthesized secondary amide compounds 3-Acetoxy-2-methyl-N-(phenyl)benzamide, I and 3-Acetoxy-2-methyl-N-(4-methylphenyl)benzamide, II. Compounds were characterized by FTIR, 1H NMR, 13C NMR and X-ray single crystal diffraction analysis techniques. Single crystal X-ray diffraction analyses show that while I crystallized in the orthorhombic system with space group Pbca, II crystallized in the triclinic system with space group P-1 and the asymmetric unit of II consists of two crystallographically independent molecules. Lattice constants are a = 7.9713 (3) Å, b = 9.5059 (3) Å, c = 37.1762 (2) Å, Z = 8 for I and a = 7.5579 (8) Å, b = 8.8601 (8) Å, c = 23.363 (3) Å, α = 97.011 (9) °, β = 96.932 (9)°, γ = 90.051 (8)°, Z = 4 for II. Crystallographic studies also show that the supramolecular structures were stabilized by intramolecular, intermolecular hydrogen bonds and Csbnd H … π interactions for both compounds. Characteristic amide bonds were observed in IR and NMR spectra.

1D cyanide complexes with 2-pyridinemethanol: Synthesis, crystal structures and spectroscopic properties

NASA Astrophysics Data System (ADS)

Sayın, Elvan; Kürkçüoğlu, Güneş Süheyla; Yeşilel, Okan Zafer; Hökelek, Tuncer

2015-12-01

Two new one-dimensional coordination polymers, [Cu(hmpH)2Pd(μ-CN)2(CN)2]n (1) and [Cu(hmpH)2Pt(μ-CN)2(CN)2]n (2), (hmpH = 2-pyridinemethanol), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. Single crystal X-ray diffraction analysis indicates that complexes 1 and 2 are isomorphous and isostructural, and crystallize in the triclinic system and P-1 space group. The Pd(II) or Pt(II) ions are four coordinated with four cyanide-carbon atoms in a square planar geometry. Cu(II) ion displays a distorted octahedral coordination by two N-atoms and two O-atoms of hmpH ligands, two bridging cyanide groups. In one dimensional structure of the complexes, [M(CN)4]2- (M = Pd(II) or Pt(II)) anions and [Cu(hmpH)2]2+ cations are linked via bridging cyanide ligands. In the complexes, the presence of intramolecular C-H⋯M (M = Pd(II) or Pt(II)) interactions with distance values of 3.00-2.95 Å are established, respectively.

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.

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.

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.

Compositional segregation and electrical properties characterization of [001]- and [011]-oriented co-growth Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 single crystal

NASA Astrophysics Data System (ADS)

Song, Kexin; Li, Zhenrong; Guo, Haisheng; Xu, Zhuo; Fan, Shiji

2018-04-01

A Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 relaxor ferroelectric single crystal boule of 3 in. diameter was grown using [001]- and [011]-oriented co-growth crystals as seeds by the modified Bridgman method. The as-grown crystal boule was divided into two growth regions [001] and [011]. The composition and the electrical properties of samples of the two regions were characterized in detail along the growth direction in the whole crystal boule. The PT content of [001]-grown samples increased from 27.7 to 36.8 mol. % along the growth direction, especially they are averagely higher about 0.7 mol. % than those of [011]-grown samples at the same growth position. The PMN content of [001]-grown samples decreased from 43.0 to 34.8 mol. %, which is lower than that of the corresponding [011]-grown samples. The compositional segregation behavior along [001] and [011] growth directions was discussed based on the crystal growth theories. Variations in the rhombohedral to tetragonal phase transition temperature (TRT), the piezoelectric properties, the coercive electric field and the remnant polarization of [001] samples were discussed according to changes in compositional segregation and crystal anisotropy. Under the exact same growth conditions, the [011]-grown crystal has a larger composition segregation effect than that of the [001]-grown crystal. This result provides a positive effect on analysing the nature and reducing the effect of compositional segregation.

Phase equilibria in the quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} and optical properties of (Ga{sub 55}In{sub 45}){sub 2}S{sub 300}, (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} single crystals

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

Ivashchenko, I.A., E-mail: Ivashchenko.Inna@eenu.edu.ua; Danyliuk, I.V.; Olekseyuk, I.D.

The quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} was investigated by differential thermal, X-ray diffraction analyses. The phase diagram of the Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} system and nine polythermal sections, isothermal section at 820 K and the liquidus surface projection were constructed. The existence of the large solid solutions ranges of binary and ternary compounds was established. The range of the existence of the quaternary phase AgGa{sub x}In{sub 5−x}S{sub 8} (2.25≤x≤2.85) at 820 K was determined. The single crystals (Ga{sub 55}In{sub 45}){sub 2}S{sub 300} and (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} were grown by a directional crystallization methodmore » from solution-melt. Optical absorption spectra in the 500–1600 nm range were recorded. The luminescence of the (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} single crystal shows a maximum at 1530 nm for the excitation wavelengths of 532 and 980 nm at 80 and 300 K. - Graphical abstract: Isothermal section of the quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} at 820 K and normalized photoluminescence spectra of the single crystal (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} at 300 K. - Highlights: • Isothermal section at 820 K, liquidus surface projection were built for Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3}. • Optical properties of single crystals were studied.« less

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.

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

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.

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.

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.

Pyrano-isoflavones with erectile-dysfunction activity from Eriosema kraussianum.

PubMed

Drewes, Siegfried E; Horn, Marion M; Munro, Orde Q; Dhlamini, Jabu T B; Meyer, J J Marion; Rakuambo, N Christopher

2002-04-01

Five pyrano-isoflavones have been isolated from the rootstock of Eriosema kraussianum N. E. Br (Papilionaceae). Spectral data and single crystal X-ray analyses were used for structural elucidation. The most active of the compounds had an activity of 75% of that found in Viagra in the erectile dysfunction test on rabbit penile smooth muscle.

Temperature-controlled two new Co(II) compounds with distinct topological networks: Syntheses, crystal structures and catalytic properties

NASA Astrophysics Data System (ADS)

Meng, Qing-Hua; Long, Xu; Liu, Jing-Li; Zhang, Shuan; Zhang, Guang-Hui

2018-04-01

Two new Co(II) coordination compounds, namely [Co2(bptc)(bpp)2]n (1) and [Co(bptc)0.5(bpp)]n (2) (H4bptc = biphenyl-3,3‧,5,5‧-tetracarboxylic acid, bpp = 1,3-di(4-pyridyl)propane), have been hydrothermally synthesized from the same reactants via tuning the reaction temperature. Single crystal X-ray diffraction analyses revealed that both 1 and 2 feature 2D sheet motifs. Topological analyses revealed that compounds 1 and 2 show distinct topological networks. Under the weak Van der Waals interactions, the 2D sheet motifs of compounds 1 and 2 are further packed into 2D→3D interdigitated supramolecular frameworks. Moreover, the two Co(II) compounds show high catalytic activities for degradation of methyl orange (MO) in a Fenten-like process.

Radiative heat transport during the vertical Bridgman growth of oxide single crystals: slabs versus cylinders

NASA Astrophysics Data System (ADS)

Virozub, Alexander; Brandon, Simon

1998-10-01

Internal radiative heat transport in oxide crystals during their growth via the vertical Bridgman technique is known to promote severely deflected melt/crystal interface shapes. These highly curved interfaces are likely to encourage unwanted phenomena such as inhomogeneous distribution of impurities in the solidified crystalline material. Past computational analyses of oxide growth systems have mostly been confined to cylindrical geometries. In this letter a two-dimensional finite-element model, describing the growth of slab-shaped oxide crystals via the vertical Bridgman technique, is presented; internal radiative heat transport through the transparent crystalline phase is accounted for in the formulation. Comparison with calculations of cylindrical-shaped crystal growth systems shows a strong dependence of thermal fields and of melt/crystal interface shapes on the crystal geometry. Specifically, the interface position is strongly shifted toward the hot zone and its curvature dramatically increases in slab-shaped systems compared to what is observed in cylindrical geometries. This significant qualitative difference in interface shapes is shown to be linked to large quantitative differences in values of the viewing angle between the hot melt/crystal interface and the cold part of the crucible.

Unique Chiral Interpenetrating d-f Heterometallic MOFs as Luminescent Sensors.

PubMed

Wu, Zhi-Lei; Dong, Jie; Ni, Wei-Yan; Zhang, Bo-Wen; Cui, Jian-Zhong; Zhao, Bin

2015-06-01

One novel three-dimensional (3D) 3d-4f metal-organic framework (MOF), [TbZn(L)(CO3)2(H2O)]n (1) [HL = 4'-(4-carboxyphenyl)-2,2':6',2″-terpyridine], has been successfully synthesized and structurally characterized. Structural analysis shows that compound 1 features a unique chiral interpenetrating 3D framework for the first time. The resulting crystals of 1 are composed of enantiomers 1a (P41) and 1b (P43), as was clearly confirmed by the crystal structure and the corresponding circular dichroism (CD) analyses of eight randomly selected crystals. The investigations on CD spectra based on every single crystal clearly assigned the Cotton effect signals. The powder X-ray diffraction measurement of 1 after being immersed in common solvents reveals that 1 possess excellent solvent stability. Furthermore, luminescent studies imply that 1 displays highly selective luminescent sensing of aldehydes, such as formol, acetaldehyde, and propanal.

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

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.

Multicomponent hydrogen-bonding organic solids constructed from 6-hydroxy-2-naphthoic acid and N-heterocycles: Synthesis, structural characterization and synthon discussion

NASA Astrophysics Data System (ADS)

Zong, Yingxia; Shao, Hui; Pang, Yanyan; Wang, Debao; Liu, Kang; Wang, Lei

2016-07-01

Seven novel multicomponent crystals involving various substituted organic amine molecules and 6-hydroxy-2-naphthoic acid were prepared and characterized by using single crystal X-ray diffraction, infrared and thermogravimetric analyses (TGA). Crystal structures with 1,4-bis(imidazol) butane (L1) 1, 1,4-bis(imidazol-1-ylmethyl)benzene (L2) 2, 1-phenyl piperazine 3, 2-amino-4-hydroxy-6-methyl pyrimidine 4, 4,4'-bipyridine 5, 5,5'-dimethyl-2,2'-dipyridine 6, 2-amino-4,6-dimethyl pyrimidine 7 were determined. Among the seven molecular complexes, total proton transfer from 6-hydroxy-2-naphthoic acid to coformer has occurred in crystals 1-4, while the remaining were cocrystals. X-ray single-crystal structures of these complexes reveal that strong hydrogen bonding O-H···O/N-H···O/O-H···N and weak C-H···O/C-H···π/π···π intermolecular interactions direct the packing modes of molecular crystals together. The analysis of supramolecular synthons in the present structures shows that some classical supramolecular synthons like pyridine-carboxylic acid heterosynthon R22 (7) and aminopyridine-carboxylic acid heterosynthon R22 (8), are again observed in constructing the hydrogen-bonding networks in this paper. Besides, we noticed that water molecules act as a significant hydrogen-bonding connector in constructing supramolecular architectures of 3, 4, 6, and 7.

Crystallization kinetics of olivine-phyric shergottites

NASA Astrophysics Data System (ADS)

Ennis, Megan E.; McSween, Harry Y.

2014-08-01

Crystal size distribution (CSD) and spatial distribution pattern (SDP) analyses are applied to the early crystallizing phases, olivine and pyroxene, in olivine-phyric shergottites (Elephant moraine [EET] 79001A, Dar al Gani [DaG] 476, and dhofar [Dho] 019) from each sampling locality inferred from Mars ejection ages. Trace element zonation patterns (P and Cr) in olivine are also used to characterize the crystallization history of these Martian basalts. Previously reported 2-D CSDs for these meteorites are re-evaluated using a newer stereographically corrected methodology. Kinks in the olivine CSD plots suggest several populations that crystallized under different conditions. CSDs for pyroxene in DaG 476 and EET 79001A reveal single populations that grew under steady-state conditions; pyroxenes in Dho 019 were too intergrown for CSD analysis. Magma chamber residence times of several days for small grains to several months for olivine megacrysts are calculated using the CSD slopes and growth rates inferred from previous experimental data. Phosphorus imaging in olivines in DaG 476 and Dho 019 indicate rapid growth of skeletal, sector-zoned, or patchy cores, probably in response to delayed nucleation, followed by slow growth, and finally rapid dendritic growth with back-filling to form oscillatory zoning in rims. SPD analyses indicate that olivine and pyroxene crystals grew or accumulated in clusters rather than as randomly distributed grains. These data reveal complex solidification histories for Martian basalts, and are generally consistent with the formation at depth of olivine megacryst cores, which were entrained in ascending magmas that crystallized pyroxenes, small olivines, and oscillatory rims on megacrysts.

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

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.

Synthesis, crystal structure and antimicrobial activities of two isomeric gold(I) complexes with nitrogen-containing heterocycle and triphenylphosphine ligands, [Au(L)(PPh3)] (HL = pyrazole and imidazole).

PubMed

Nomiya, K; Noguchi, R; Ohsawa, K; Tsuda, K; Oda, M

2000-03-01

Two isomeric gold(I)-triphenylphosphine complexes with nitrogen-containing heterocycles, [Au(L)(PPh3) (HL = pyrazole (1), imidazole (2)) were isolated as colorless cubic crystals for 1 and colorless plate crystals for 2, respectively. The crystal structures of 1 and 2 were determined by single-crystal X-ray diffraction. These complexes were also fully characterized by complete elemental analyses, thermogravimetric/differential thermal analyses (TG/DTA) and FT-IR in the solid state and by solution NMR (31P, 1H and 13C) spectroscopy and molecular weight measurements in acetone solution. These complexes consisted of a monomeric 2-coordinate AuNP core both in the solid state and in solution. The molecular structures of 1 and 2 were compared with those of related gold(I) complexes, [Au(1,2,3-triz)(PPh3)] (3, Htriz = triazole), [Au(1,2,4-triz)(PPh3)]2 (4) as a dimer through a gold(I)-gold(I) bond in the solid state, and [Au(tetz)(PPh3)] (5, Htetz = tetrazole). Selective and effective antimicrobial activities against two gram-positive bacteria (B. subtilis, S. aureus) and modest activities against one yeast (C. albicans) found in these gold(I) complexes 1-4 are noteworthy, in contrast to poor activities observed in the corresponding silver(I) complexes.

Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

PubMed

Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

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.

Age of the Lava Creek supereruption and magma chamber assembly at Yellowstone based on 40Ar/39Ar and U-Pb dating of sanidine and zircon crystals

USGS Publications Warehouse

Matthews, Naomi E.; Vazquez, Jorge A.; Calvert, Andrew T.

2015-01-01

The last supereruption from the Yellowstone Plateau formed Yellowstone caldera and ejected the >1000 km3 of rhyolite that composes the Lava Creek Tuff. Tephra from the Lava Creek eruption is a key Quaternary chronostratigraphic marker, in particular for dating the deposition of mid Pleistocene glacial and pluvial deposits in western North America. To resolve the timing of eruption and crystallization history for the Lava Creek magma, we performed (1) 40Ar/39Ar dating of single sanidine crystals to delimit eruption age and (2) ion microprobe U-Pb and trace-element analyses of the crystal faces and interiors of single zircons to date the interval of zircon crystallization and characterize magmatic evolution. Sanidines from the two informal members composing Lava Creek Tuff yield a preferred 40Ar/39Ar isochron date of 631.3 ± 4.3 ka. Crystal faces on zircons from both members yield a weighted mean 206Pb/238U date of 626.5 ± 5.8 ka, and have trace element concentrations that vary with the eruptive stratigraphy. Zircon interiors yield a mean 206Pb/238U date of 659.8 ± 5.5 ka, and reveal reverse and/or oscillatory zoning of trace element concentrations, with many crystals containing high U concentration cores that likely grew from highly evolved melt. The occurrence of distal Lava Creek tephra in stratigraphic sequences marking the Marine Isotope Stage 16–15 transition supports the apparent eruption age of ∼631 ka. The combined results reveal that Lava Creek zircons record episodic heating, renewed crystallization, and an overall up-temperature evolution for Yellowstone's subvolcanic reservoir in the 103−104 year interval before eruption.

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.

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.

Inorganic pyrophosphatase crystals from Thermococcus thioreducens for X-ray and neutron diffraction.

PubMed

Hughes, Ronny C; Coates, Leighton; Blakeley, Matthew P; Tomanicek, Steve J; Langan, Paul; Kovalevsky, Andrey Y; García-Ruiz, Juan M; Ng, Joseph D

2012-12-01

Inorganic pyrophosphatase (IPPase) from the archaeon Thermococcus thioreducens was cloned, overexpressed in Escherichia coli, purified and crystallized in restricted geometry, resulting in large crystal volumes exceeding 5 mm3. IPPase is thermally stable and is able to resist denaturation at temperatures above 348 K. Owing to the high temperature tolerance of the enzyme, the protein was amenable to room-temperature manipulation at the level of protein preparation, crystallization and X-ray and neutron diffraction analyses. A complete synchrotron X-ray diffraction data set to 1.85 Å resolution was collected at room temperature from a single crystal of IPPase (monoclinic space group C2, unit-cell parameters a=106.11, b=95.46, c=113.68 Å, α=γ=90.0, β=98.12°). As large-volume crystals of IPPase can be obtained, preliminary neutron diffraction tests were undertaken. Consequently, Laue diffraction images were obtained, with reflections observed to 2.1 Å resolution with I/σ(I) greater than 2.5. The preliminary crystallographic results reported here set in place future structure-function and mechanism studies of IPPase.

Two novel transition metal-organic frameworks based on 1,3,5-benzenetricarboxylate ligand: Syntheses, structures and thermal properties

NASA Astrophysics Data System (ADS)

Fu, Ying; Li, Guobao; Liao, Fuhui; Xiong, Ming; Lin, Jianhua

2011-10-01

Two novel transition metal-organic frameworks, [Zn 6(OH) 3(BTC) 3(H 2O) 3]ṡ7H 2O ( 1) and [Cd(BTC)(H 2O)]ṡ[HIM] ( 2) (H 3BTC = 1,3,5-benzenetricarboxylic acid), have been synthesized under hydrothermal conditions and characterized by single crystal and variable temperature powder X-ray diffraction (VTPXRD), IR spectroscopy, elemental analyses, ICP measurements, and coupled TG-MS analyses. Compound 1 crystallizes in the trigonal space group R3 c, and could be described as a 3D porous network consisting of (Zn 2O 8) n zigzag chains and bridging BTC ligands with 1D channels along c axis. Compound 2 crystallizes in the monoclinic space group P2 1/ c, and exhibits a 2D framework made up of CdO 6 octahedra and BTC ligands parallel the bc plane. TG-MS and VTPXRD studies reveal that 1 is stable up to 320 °C under air, and 2 stable up to 220 °C.

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.

Crystal growth, structural, optical, thermal and dielectric properties of lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

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

2017-11-01

The vibrational groups of the lithium hydrogen oxalate monohydrate have been investigated by FTIR and FT- Raman analyses. It has low absorbance in the UV-Vis-NIR region. The laser damage threshold study confirms that the material withstands upto 30 mJ with time of 7 s, after that circular dot damage is seen on the surface. The dark region of the surface damage spot occurs due to the thermal effects. The material is thermally stable upto 93 °C and there is no weight loss below this temperature. The dielectric studies were carried out at the frequency regions of 1 kHz-1 MHz and different temperatures from 40 °C to 80 °C. Semi-organic non-linear optical (NLO) single crystal lithium hydrogen oxalate monohydrate has been grown by slow evaporation solution growth technique. The Hirshfeld surface analysis was performed to understand the different intermolecular interactions in the title compound. The fingerprint plots contain the highest portion of H⋯O/O⋯H (48.3%) interactions.

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.

Tribological properties of sintered polycrystalline and single crystal silicon carbide

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.; Srinivasan, M.

1982-01-01

Tribological studies and X-ray photoelectron spectroscopy analyses were conducted with sintered polycrystalline and single crystal silicon carbide surfaces in sliding contact with iron at various temperatures to 1500 C in a vacuum of 30 nPa. The results indicate that there is a significant temperature influence on both the friction properties and the surface chemistry of silicon carbide. The main contaminants on the as received sintered polycrystalline silicon carbide surfaces are adsorbed carbon, oxygen, graphite, and silicon dioxide. The surface revealed a low coefficient of friction. This is due to the presence of the graphite on the surface. At temperatures of 400 to 600 C graphite and copious amount of silicon dioxide were observed on the polycrystalline silicon carbide surface in addition to silicon carbide. At 800 C, the amount of the silicon dioxide decreased rapidly and the silicon carbide type silicon and carbon peaks were at a maximum intensity in the XPS spectra. The coefficients of friction were high in the temperature range 400 to 800 C. Small amounts of carbon and oxygen contaminants were observed on the as received single crystal silicon carbide surface below 250 C. Silicon carbide type silicon and carbon peaks were seen on the silicon carbide in addition to very small amount of graphite and silicon dioxide at temperatures of 450 to 800 C.

Anderson localization of electrons in single crystals: LixFe7Se8

PubMed Central

Ying, Tianping; Gu, Yueqiang; Chen, Xiao; Wang, Xinbo; Jin, Shifeng; Zhao, Linlin; Zhang, Wei; Chen, Xiaolong

2016-01-01

Anderson (disorder-induced) localization, proposed more than half a century ago, has inspired numerous efforts to explore the absence of wave diffusions in disordered media. However, the proposed disorder-induced metal-insulator transition (MIT), associated with the nonpropagative electron waves, has hardly been observed in three-dimensional (3D) crystalline materials, let alone single crystals. We report the observation of an MIT in centimeter-size single crystals of LixFe7Se8 induced by lattice disorder. Both specific heat and infrared reflectance measurements reveal the presence of considerable electronic states in the vicinity of the Fermi level when the MIT occurs, suggesting that the transition is not due to Coulomb repulsion mechanism. The 3D variable range hopping regime evidenced by electrical transport measurements at low temperatures indicates the localized nature of the electronic states on the Fermi level. Quantitative analyses of carrier concentration, carrier mobility, and simulated density of states (DOS) fully support that LixFe7Se8 is an Anderson insulator. On the basis of these results, we provide a unified DOS picture to explain all the experimental results, and a schematic diagram for finding other potential Anderson insulators. This material will thus serve as a rich playground for both theoretical and experimental investigations on MITs and disorder-induced phenomena. PMID:26989781

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.

Growth and microtopographic study of CuInSe{sub 2} single crystals

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

Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P.

2016-05-23

The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

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.

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

High Strain Rate and Shock-Induced Deformation in Metals

NASA Astrophysics Data System (ADS)

Ravelo, Ramon

2012-02-01

Large-scale non-equilibrium molecular Dynamics (MD) simulations are now commonly used to study material deformation at high strain rates (10^9-10^12 s-1). They can provide detailed information-- such as defect morphology, dislocation densities, and temperature and stress profiles, unavailable or hard to measure experimentally. Computational studies of shock-induced plasticity and melting in fcc and bcc single, mono-crystal metals, exhibit generic characteristics: high elastic limits, large directional anisotropies in the yield stress and pre-melting much below the equilibrium melt temperature for shock wave propagation along specific crystallographic directions. These generic features in the response of single crystals subjected to high strain rates of deformation can be explained from the changes in the energy landscape of the uniaxially compressed crystal lattice. For time scales relevant to dynamic shock loading, the directional-dependence of the yield strength in single crystals is shown to be due to the onset of instabilities in elastic-wave propagation velocities. The elastic-plastic transition threshold can accurately be predicted by a wave-propagation stability analysis. These strain-induced instabilities create incipient defect structures, which can be quite different from the ones, which characterize the long-time, asymptotic state of the compressed solid. With increase compression and strain rate, plastic deformation via extended defects gives way to amorphization associated with the loss in shear rigidity along specific deformation paths. The hot amorphous or (super-cooled liquid) metal re-crystallizes at rates, which depend on the temperature difference between the amorphous solid and the equilibrium melt line. This plastic-amorphous transition threshold can be computed from shear-waves stability analyses. Examples from selected fcc and bcc metals will be presented employing semi-empirical potentials of the embedded atom method (EAM) type as well as results from density functional theory calculations.

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.

Surface and subsurface cracks characteristics of single crystal SiC wafer in surface machining

NASA Astrophysics Data System (ADS)

Qiusheng, Y.; Senkai, C.; Jisheng, P.

2015-03-01

Different machining processes were used in the single crystal SiC wafer machining. SEM was used to observe the surface morphology and a cross-sectional cleavages microscopy method was used for subsurface cracks detection. Surface and subsurface cracks characteristics of single crystal SiC wafer in abrasive machining were analysed. The results show that the surface and subsurface cracks system of single crystal SiC wafer in abrasive machining including radial crack, lateral crack and the median crack. In lapping process, material removal is dominated by brittle removal. Lots of chipping pits were found on the lapping surface. With the particle size becomes smaller, the surface roughness and subsurface crack depth decreases. When the particle size was changed to 1.5µm, the surface roughness Ra was reduced to 24.0nm and the maximum subsurface crack was 1.2µm. The efficiency of grinding is higher than lapping. Plastic removal can be achieved by changing the process parameters. Material removal was mostly in brittle fracture when grinding with 325# diamond wheel. Plow scratches and chipping pits were found on the ground surface. The surface roughness Ra was 17.7nm and maximum subsurface crack depth was 5.8 µm. When grinding with 8000# diamond wheel, the material removal was in plastic flow. Plastic scratches were found on the surface. A smooth surface of roughness Ra 2.5nm without any subsurface cracks was obtained. Atomic scale removal was possible in cluster magnetorheological finishing with diamond abrasive size of 0.5 µm. A super smooth surface eventually obtained with a roughness of Ra 0.4nm without any subsurface crack.

Giant increase of critical current density and vortex pinning in Mn doped K{sub x}Fe{sub 2−y}Se{sub 2} single crystals

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

Li, Mingtao; Zhang, Jincang, E-mail: jczhang@staff.shu.edu.cn; Materials Genome Institute, Shanghai University, Shanghai 200444

2014-11-10

We report a comparative study of the critical current density (J{sub c}) and vortex pinning among pure and Mn doped K{sub x}Fe{sub 2−y}Se{sub 2} single crystals. It is found that the J{sub c} values can be greatly improved by Mn doping and post-quenching treatment when comparing to pristine pure sample. In contrast to pure samples, an anomalous second magnetization peak (SMP) effect is observed in both 1% and 2% Mn doped samples at T = 3 K for H∥ab but not for H∥c. Referring to Dew-Hughes and Kramer's model, we performed scaling analyses of the vortex pinning force density vs magnetic field inmore » 1% Mn doped and quenched pristine crystals. The results show that the normal point defects are the dominant pinning sources, which probably originate from the variations of intercalated K atoms. We propose that the large nonsuperconducting K-Mn-Se inclusions may contribute to the partial normal surface pinning and give rise to the anomalous SMP effect for H∥ab in Mn doped crystals. These results may facilitate further understanding of the superconductivity and vortex pinning in intercalated iron-selenides superconductors.« less

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

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.

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.

On the colour of wing scales in butterflies: iridescence and preferred orientation of single gyroid photonic crystals.

PubMed

Corkery, Robert W; Tyrode, Eric C

2017-08-06

Lycaenid butterflies from the genera Callophrys , Cyanophrys and Thecla have evolved remarkable biophotonic gyroid nanostructures within their wing scales that have only recently been replicated by nanoscale additive manufacturing. These nanostructures selectively reflect parts of the visible spectrum to give their characteristic non-iridescent, matte-green appearance, despite a distinct blue-green-yellow iridescence predicted for individual crystals from theory. It has been hypothesized that the organism must achieve its uniform appearance by growing crystals with some restrictions on the possible distribution of orientations, yet preferential orientation observed in Callophrys rubi confirms that this distribution need not be uniform. By analysing scanning electron microscope and optical images of 912 crystals in three wing scales, we find no preference for their rotational alignment in the plane of the scales. However, crystal orientation normal to the scale was highly correlated to their colour at low (conical) angles of view and illumination. This correlation enabled the use of optical images, each containing up to 10 4 -10 5 crystals, for concluding the preferential alignment seen along the [Formula: see text] at the level of single scales, appears ubiquitous. By contrast, [Formula: see text] orientations were found to occur at no greater rate than that expected by chance. Above a critical cone angle, all crystals reflected bright green light indicating the dominant light scattering is due to the predicted band gap along the [Formula: see text] direction, independent of the domain orientation. Together with the natural variation in scale and wing shapes, we can readily understand the detailed mechanism of uniform colour production and iridescence suppression in these butterflies. It appears that the combination of preferential alignment normal to the wing scale, and uniform distribution within the plane is a near optimal solution for homogenizing the angular distribution of the [Formula: see text] band gap relative to the wings. Finally, the distributions of orientations, shapes, sizes and degree of order of crystals within single scales provide useful insights for understanding the mechanisms at play in the formation of these biophotonic nanostructures.

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.

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

Thermal-structural analyses of Space Shuttle Main Engine (SSME) hot section components

NASA Technical Reports Server (NTRS)

Abdul-Aziz, Ali; Thompson, Robert L.

1988-01-01

Three dimensional nonlinear finite element heat transfer and structural analyses were performed for the first stage high pressure fuel turbopump (HPFTP) blade of the space shuttle main engine (SSME). Directionally solidified (DS) MAR-M 246 and single crystal (SC) PWA-1480 material properties were used for the analyses. Analytical conditions were based on a typical test stand engine cycle. Blade temperature and stress strain histories were calculated by using the MARC finite element computer code. The structural response of an SSME turbine blade was assessed and a greater understanding of blade damage mechanisms, convective cooling effects, and thermal mechanical effects was gained.

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

Raman Spectroscopy of Rdx Single Crystals Under Static Compression

NASA Astrophysics Data System (ADS)

Dreger, Zbigniew A.; Gupta, Yogendra M.

2007-12-01

To gain insight into the high pressure response of energetic crystal of RDX, Raman measurements were performed under hydrostatic compression up to 15 GPa. Several distinct changes in the spectra were found at 4.0±0.3 GPa, confirming the α-γ phase transition previously observed in polycrystalline samples. Symmetry correlation analyses indicate that the γ-polymorph may assume a space group isomorphous with a point group D2h with eight molecules occupying the C1 symmetry sites, similar to the α-phase. It is proposed that factor group coupling can account for the observed increase in the number of modes in the γ-phase.

Photorefractive detection of tagged photons in ultrasound modulated optical tomography of thick biological tissues.

PubMed

Ramaz, F; Forget, B; Atlan, M; Boccara, A C; Gross, M; Delaye, P; Roosen, G

2004-11-01

We present a new and simple method to obtain ultrasound modulated optical tomography images in thick biological tissues with the use of a photorefractive crystal. The technique offers the advantage of spatially adapting the output speckle wavefront by analysing the signal diffracted by the interference pattern between this output field and a reference beam, recorded inside the photorefractive crystal. Averaging out due to random phases of the speckle grains vanishes, and we can use a fast single photodetector to measure the ultrasound modulated optical contrast. This technique offers a promising way to make direct measurements within the decorrelation time scale of living tissues.

Unconventional Magnetic Domain Structure in the Ferromagnetic Phase of MnP Single Crystals

NASA Astrophysics Data System (ADS)

Koyama, Tsukasa; Yano, Shin-ichiro; Togawa, Yoshihiko; Kousaka, Yusuke; Mori, Shigeo; Inoue, Katsuya; Kishine, Jun-ichiro; Akimitsu, Jun

2012-04-01

We have studied ferromagnetic (FM) structures in the FM phase of MnP single crystals by low-temperature Lorentz transmission electron microscopy and small-angle electron diffraction analysis. In Lorentz Fresnel micrographs, striped FM domain structures were observed at an external magnetic field less than 10 Oe in specimens with the ab-plane in their plane. From real- and reciprocal-space analyses, it was clearly identified that striped FM domains oriented to the c-axis appear with Bloch-type domain walls in the b-direction and order regularly along the a-axis with a constant separation less than 100 nm. Moreover, the magnetic chirality reverses in alternate FM domain walls. These specific spin configuration of striped FM domains will affect the magnetic phase transition from the FM phase to the proper screw spiral phase at low temperature or to the FAN phase in magnetic fields in MnP.

Geochemistry, thermometry and isotope ratios on the same zircon crystals: the tandem use of quadrupole LA-ICPMS and CA-TIMS

NASA Astrophysics Data System (ADS)

Olin, P. H.; Schmitz, M. D.; Crowley, J. L.

2011-12-01

Current trends in igneous petrology include the extraction of diverse geochemical information from smaller sample targets by ever more efficient and cost effective means. Igneous zircons are repositories of several types of petrogenetic information, such as magmatic crystallization ages obtained using U-Pb geochronology, magmatic temperatures using Ti-in-zircon geothermometry, and magmatic differentiation and/or mixing trends using trace element contents. Here we demonstrate a tandem quadrupole LA-ICPMS and CA-TIMS approach on single zircon crystals and within domains in single crystals, which extracts all of these data from a single laser spot analysis and then guides the acquisition of CA-TIMS ages at precisions relevant to magmatic histories. We present data from zircon-bearing intrusive and extrusive rocks spanning the compositional spectrum, and highlight results from silicic volcanic rocks with different affinities. The utility of our approach is illustrated in zircons from the Temora diorite, a commonly used standard material which we analysed using 25-μm ablation spots placed on dozens of grains which had been previously annealed and chemically abraded prior to mounting in epoxy. Our LA-ICPMS results illustrate a 3- to 5-fold variation in trace element concentrations and trace element ratios over >150 degrees of cooling as estimated from Ti-in-zircon thermometry. Some geochemical parameters (e.g., Nb/Ta variations and Eu anomalies) are consistent with crystal fractionation during progressive crystallization, while others are bimodal (e.g., Hf and U contents), suggesting the mixing of crystal/magma batches prior to final solidification. LA-ICPMS U-Pb spot ages reproduce the accepted CA-TIMS age within 2% precision and accuracy, while our CA-TIMS results on the same grains constrain the development of the observed geochemical variability to within 100 ka. Other zircon standard materials to be presented include Plesovich syenite, FC1 gabbro, and R33 diorite. Analyses of zircons from selected western Snake River Plain silicic volcanic units further demonstrate the capability of our approach. These units are targeted with the overarching goal of better understanding magmatism in the region and to identify geochemical fingerprints to better distinguish among and to correlate between units. Several rhyolites distributed along the northern margin of the plain have LA-ICPMS ages of ca. 11 Ma, within error of each other and their CA-TIMS ages, and reveal differences in temperatures of crystallization and trace element contents and ratios. Individual units have crystallization temperatures that span 100 degrees or more, and show correlations with whole-rock major and trace element contents and ratios. In many cases, zircon geochemical parameters such as REE and Y contents, and Nb/Ta and Th/U ratios allow units proximal to each other to be distinguished from one another while also providing fingerprints to correlate to distal units on the south side of the plain or elsewhere in the province.

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.

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).

Effect of L-Valine on the growth and characterization of Sodium Acid Phthalate (SAP) single crystals.

PubMed

Nirmala, L Ruby; Thomas Joseph Prakash, J

2013-06-01

Undoped and amino acid doped good quality single crystals of Sodium Acid Phthalate crystals (SAP) were grown by slow evaporation solution growth technique which are semiorganic in nature. The effect of amino acid (L-Valine) dopant on the growth and the properties of SAP single crystal was investigated. The single crystal X-ray diffraction studies and FT-IR studies were carried out to identify the crystal structure and the presence of functional groups in undoped and L-Valine doped SAP crystals. The transparent nature of the grown crystal was observed using UV-Visible spectrum. The thermal decomposition of the doped SAP crystals was investigated by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). The enhancement in the NLO property of the undoped and L-Valine doped SAP crystals using KDP crystal as a reference was studied using SHG measurements. Vickers micro hardness measurements are used for the study of mechanical strength of the grown crystals. Copyright © 2013 Elsevier B.V. All rights reserved.

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

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.

Crystal growth, structure analysis and characterisation of 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid single crystal

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

Sankari, R. Siva, E-mail: sivasankari.sh@act.edu.in; Perumal, Rajesh Narayana

2014-04-24

Single crystal of dielectric material 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid has been grown by slow evaporation solution growth method. The grown crystal was harvested in 25 days. The crystal structure was analyzed by Single crystal X - ray diffraction. UV-vis-NIR analysis was performed to examine the optical property of the grown crystal. The thermal property of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The dielectric measurements were carried out and the dielectric constant was calculated and plotted at all frequencies.

A Study of the Synchrotron Laue Method for Quantitative Crystal Structure Analysis

NASA Astrophysics Data System (ADS)

Gomez de Anderez, Dora M.

1990-01-01

Quantitative crystal structure analyses have been carried out on small molecule crystals using synchrotron radiation and the Laue method. A variety of single crystal structure determinations and associated refinements are used and compared with the monochromatic analyses. The new molecular structure of 7-amino-5-bromo -4-methyl-2-oxo-1,2,3,4 -tetrahidro-1,6 -naphthyridine-8-carbonitrile (C_{10 }H_9ON_4 BrcdotH_2O) has been determined, first using monochromatic Mo K alpha radiation and a four-circle diffractometer, then using synchrotron Laue diffraction photography. The structure refinements showed an R-factor of 4.97 and 14.0% for the Mo Kalpha and Laue data respectively. The molecular structure of (S)-2-chloro-2-fluoro-N-((S)-1-phenylethyl) ethanamide, (C_{10}H _{11}ClFNO), has been determined using the same crystal throughout for X-ray monochromatic analyses (Mo Kalpha and Cu K alpha) followed by synchrotron Laue data collection. The Laue and monochromatic data compare favourably. The R -factors (on F) were 6.23, 6.45 and 8.19% for the Mo K alpha, Cu Kalpha and Laue data sets respectively. The molecular structure of 3-(5-hydroxy-3-methyl-1-phenylpyrazol-4-yl)-1,3-diphenyl -prop-2-en-1-one, (C_{25}H _{20}N_2 O_2) has been determined using the synchrotron Laue method. The results compare very well with Mo Kalpha monochromatic data. The R-factors (on F) were 4.60 and 5.29% for Mo Kalpha and Laue analyses respectively. The Laue method is assessed in locating the 20 hydrogen atoms in this structure. The structure analyses of the benzil compound ((C_6H_5 OcdotCO_2)) is carried out using the synchrotron Laue method firstly at room temperature and secondly at low temperature. The structure shows an R-factor (on F) of 13.06% and 6.85% for each data set respectively. The synchrotron Laue method was used to collect data for ergocalciferol (Vitamin D_2). The same crystal was also used to record oscillation data with the synchrotron radiation monochromatic beam. A new molecular structure of (Dinitrato-(N,N ^'-dimethylethylene-diamine)copper(II)) has been determined using Mo Kalpha radiation on a four circle diffractometer. The refinement resulted in an R-factor (on F) of 4.06%.

Three reversible polymorphic copper(I) complexes triggered by ligand conformation: insights into polymorphic crystal habit and luminescent properties.

PubMed

Chai, Wenxiang; Hong, Mingwei; Song, Li; Jia, Guohua; Shi, Hongsheng; Guo, Jiayu; Shu, Kangying; Guo, Bing; Zhang, Yicheng; You, Wenwu; Chen, Xueyuan

2015-05-04

Three luminescent polymorphs based on a new copper(I) complex Cu(2-QBO)(PPh3)PF6 (1, PPh3 = triphenylphosphine, 2-QBO = 2-(2'-quinolyl)benzoxazole) have been synthesized and characterized by FT-IR, UV-vis, elemental analyses, and single-crystal X-ray diffraction analyses. Each polymorph can reversibly convert from one to another through appropriate procedures. Interestingly, such interconversion can be distinguished by their intrinsic crystal morphologies and colors (namely α, dark yellow plate, β, orange block, γ, light yellow needle) as well as photoluminescent (PL) properties. X-ray crystal structure analyses of these three polymorphs show three different supramolecular structures from 1D to 3D, which are expected to be responsible for the formation of three different crystal morphologies such as needle, plate, and block. Combination of the experimental data with DFT calculations on these three polymorphs reveals that the polymorphic interconversion is triggered by the conformation isomerization of the 2-QBO ligand and can be successfully controlled by the polarity of the process solvents (affecting the molecular dipole moment) and thermodynamics (affecting the molecular total energy). It is also found that the different crystal colors of polymorphs and their PL properties are derived from different θ values (dihedral angle between benzoxazolyl and quinolyl group of the 2-QBO ligand) and P-Cu-P angles based on TD-DFT calculations. Moreover, an interesting phase interconversion between γ and β has also been found under different temperature, and this result is consistent with the DFT calculations in which the total energy of β is larger than that of γ. This polymorphism provides a good model to study the relationship between the structure and the physical properties in luminescent copper(I) complexes as well as some profound insights into their PL properties.

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.

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.

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

Structural, optical, mechanical and dielectric studies of pure and doped L-Prolinium trichloroacetate single crystals.

PubMed

Renuka, N; Ramesh Babu, R; Vijayan, N; Vasanthakumar, Geetha; Krishna, Anuj; Ramamurthi, K

2015-02-25

In the present work, pure and metal substituted L-Prolinium trichloroacetate (LPTCA) single crystals were grown by slow evaporation method. The grown crystals were subjected to single crystal X-ray diffraction (XRD), powder X-ray diffraction, FTIR, UV-Visible-NIR, hardness, photoluminescence and dielectric studies. The dopant concentration in the crystals was measured by inductively coupled plasma (ICP) analysis. Single crystal X-ray diffraction studies of the pure and metal substituted LPTCA revealed that the grown crystals belong to the trigonal system. Ni(2+) and Co(2+) doping slightly altered the lattice parameters of LPTCA without affecting the basic structure of the crystal. FTIR spectral analysis confirms the presence of various functional groups in the grown crystals. The mechanical behavior of pure and doped crystals was analyzed by Vickers's microhardness test. The optical transmittance, dielectric and photoluminescence properties of the pure and doped crystals were analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

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 and magnetostrictive behavior of Dy 3+ doped CoFe 2O 4 single crystals grown by flux method

NASA Astrophysics Data System (ADS)

Kambale, Rahul C.; Song, K. M.; Won, C. J.; Lee, K. D.; Hur, N.

2012-02-01

We studied the effect of Dy 3+ content on the magnetic properties of cobalt ferrite single crystal. The single crystals of CoFe 1.9Dy 0.1O 4 were grown by the flux method using Na 2B 4O 7.10 H 2O (Borax) as a solvent (flux). The black and shiny single crystals were obtained as a product. The X-ray diffraction analysis at room temperature confirmed the spinel cubic structure with lattice constant a=8.42 Å of the single crystals. The compositional analysis endorses the presence of constituents Co, Fe and Dy elements after sintering at 1300 °C within the final structure. The magnetic hysteresis measurements at various temperatures viz. 10 K, 100 K, 200 K and 300 K reveal the soft ferrimagnetic nature of the single crystal than that of for pure CoFe 2O 4. The observed saturation magnetization ( Ms) and coercivity ( Hc) are found to be lower than that of pure CoFe 2O 4 single crystal. The magnetostriction ( λ) measurement was carried out along the [001] direction. The magnetic measurements lead to conclude that the present single crystals can be used for magneto-optic recording media.

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.

In Situ TEM and AFM Investigation of Morphological Controls during the Growth of Single Crystal BaWO 4

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

Liu, Lili; Zhang, Shuai; Bowden, Mark E.

Barium tungstate (BaWO 4) is a widely investigated inorganic optical material due to its attractive emission properties. Because those properties strongly depend on crystal structure and morphology, numerous approaches to controlling growth have been pursued. However, an understanding of the growth mechanisms that lead to the wide range of morphologies obtained to date is largely lacking, and most attempts to develop that understanding have been based on post-growth analyses. Significantly, such analyses have led to the conclusion that certain BaWO 4 crystal morphologies result from a nonclassical growth process of oriented attachment. In this work, we systematically varied the morphologymore » of BaWO 4 crystals by adjusting the relative concentrations of solute, water, and ethanol. We then explored the growth mechanism leading to the observed range of morphologies through in situ TEM and in situ AFM. We find that even the most complex BaWO 4 morphologies occur through purely classical growth mechanisms largely controlled by the content of solute and ethanol. The latter acts as an impurity to poison growth at low concentrations and low solute levels, but leads to development of growth instabilities and eventual dendritic growth at high alcohol and moderate solute concentrations by driving up the supersaturation. These findings also highlight the necessity of in situ experiments to interpret ex situ observations of crystal growth and decipher the controlling mechanisms.« less

Crystal growth, structural, spectral, thermal, dielectric, linear and nonlinear optical characteristics of a new organic acentric material: L-Methionine-Succinic acid (2/1)

NASA Astrophysics Data System (ADS)

Nageshwari, M.; Kumari, C. Rathika Thaya; Vinitha, G.; Mohamed, M. Peer; Sudha, S.; Caroline, M. Lydia

2018-03-01

L-Methionine-Succinic acid (2/1) (LMSA), 2C5H11NO2S·C4H6O4, a novel nonlinear optical material which belongs to the class of organic category was grown-up for the first time by the technique of slow evaporation. Purity of LMSA was improved using repetitive recrystallization. LMSA was analyzed by single crystal and powder X-ray diffraction investigation to affirm the crystal structure and crystalline character. The single crystal XRD revealed that LMSA corresponds to the crystal system of triclinic with P1 as space group showing the asymmetric unit consists of a neutral succinic acid molecule and two methionine residues which are crystallographically independent existing in zwitterionic form. The functional groups existing in LMSA was accomplished using Fourier transform infrared spectroscopy. The optical transparency and the band gap energy were identified utilizing UV-Visible spectrum. The optical constants specifically reflectance and extinction coefficient clearly indicate the elevated transparency of LMSA. The thermal analyses affirmed its thermal stability. The luminescence behavior of LMSA has been analyzed by Photoluminescence (PL) spectral study. The mechanical, laser damage threshold and dielectric investigation of LMSA was done to suggest the material for practical applications. The second and third harmonic generation efficacy was confirmed by means of Kurtz-Perry and Z-scan procedure which attest its potentiality in the domain of nonlinear optics.

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.

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.

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.

Complete titanium substitution by boron in a tetragonal prism: exploring the complex boride series Ti(3-x)Ru(5-y)Ir(y)B(2+x) (0 ≤ x ≤ 1 and 1 < y < 3) by experiment and theory.

PubMed

Fokwa, Boniface P T; Hermus, Martin

2011-04-18

Polycrystalline samples and single crystals of four members of the new complex boride series Ti(3-x)Ru(5-y)Ir(y)B(2+x) (0 ≤ x ≤ 1 and 1 < y < 3) were synthesized by arc-melting the elements in a water-cooled copper crucible under an argon atmosphere. The new silvery phases were structurally characterized by powder and single-crystal X-ray diffraction as well as energy- and wavelength-dispersive X-ray spectroscopy analyses. They crystallize with the tetragonal Ti(3)Co(5)B(2) structure type in space group P4/mbm (No. 127). Tetragonal prisms of Ru/Ir atoms are filled with titanium in the boron-poorest phase (Ti(3)Ru(2.9)Ir(2.1)B(2)). Gradual substitution of titanium by boron then results in the successive filling of this site by a Ti/B mixture en route to the complete boron occupation, leading to the boron-richest phase (Ti(2)Ru(2.8)Ir(2.2)B(3)). Furthermore, both ruthenium and iridium share two sites in these structures, but a clear Ru/Ir site preference is found. First-principles density functional theory calculations (Vienna ab initio simulation package) on appropriate structural models (using a supercell approach) have provided more evidence on the stability of the boron-richest and -poorest phases, and the calculated lattice parameters corroborate very well with the experimentally found ones. Linear muffin-tin orbital atomic sphere approximation calculations further supported these findings through crystal orbital Hamilton population bonding analyses, which also show that the Ru/Ir-B and Ru/Ir-Ti heteroatomic interactions are mainly responsible for the structural stability of these compounds. Furthermore, some stable and unstable phases of this complex series could be predicted using the rigid-band model. According to the density of states analyses, all phases should be metallic conductors, as was expected from these metal-rich borides.

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.

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

Preparation and guest-uptake protocol for a porous complex useful for 'crystal-free' crystallography.

PubMed

Inokuma, Yasuhide; Yoshioka, Shota; Ariyoshi, Junko; Arai, Tatsuhiko; Fujita, Makoto

2014-02-01

We recently reported a new method for single-crystal X-ray diffraction (SCD) analysis that does not require the crystallization of the target compound. In this 'crystal-free' crystallography, a tiny crystal of a porous complex is soaked in the solution of the target guest. The guest molecules are absorbed and oriented in the crystal pores and can be analyzed by X-ray diffraction. We describe here a detailed synthetic protocol for the preparation of uniform single crystals of the porous host complex and for the subsequent guest uptake. The protocol describes our most versatile porous complex, which is prepared from commercially available ZnI2 and 2,4,6-tri(4-pyridyl)-1,3,5-triazine. The host complex has large pores with a cross-section of 8 × 5 Å(2). Single crystals of the complex are grown from layered solutions of the two components. The pores of the as-synthesized complex are filled with nitrobenzene, which is replaced with the inert solvent cyclohexane. This solvent exchange is essential for the rapid and effective inclusion of target compounds. The most crucial and delicate step is the selection of high-quality single crystals from the mixture of crystals of various shapes and sizes. We suggest using the facial indices of the single crystals as a criterion for crystal selection. Single-crystal samples for X-ray analysis can be prepared by immersing the selected crystals in a cyclohexane/dichloromethane solution of target compound. After a very slow evaporation of the solvent, typically over 2 d, the final crystal can be picked and directly subjected to SCD analysis. The protocol can be completed within ∼16 d.

Liquid crystal nanocomposites produced by mixtures of hydrogen bonded achiral liquid crystals and functionalized carbon nanotubes

NASA Astrophysics Data System (ADS)

Katranchev, B.; Petrov, M.; Keskinova, E.; Naradikian, H.; Rafailov, P. M.; Dettlaff-Weglikowska, U.; Spassov, T.

2014-12-01

The liquid crystalline (LC) nature of alkyloxybenzoic acids is preserved after adding of any mesogenic or non-mesogenic compound through hydrogen bonding. However, this noncovalent interaction provokes a sizable effect on the physical properties as, e. g. melting point and mesomorphic states. In the present work we investigate nanocomposites, prepared by mixture of the eighth homologue of p-n-alkyloxybenzoic acids (8OBA) with single-walled carbon nanotubes (SWCNT) with the purpose to modify the optical properties of the liquid crystal. We exercise optical control on the LC system by inserting SWCNT specially functionalized by carboxylic groups. Since the liquid crystalline state combines order and mobility at the molecular (nanoscale) level, molecular modification can lead to different macroscopical nanocomposite symmetry. The thermal properties of the functionalized nanocomposite are confirmed by DSC analyses. The mechanism of the interaction between surface-treated nanoparticles (functionalized nanotubes) and the liquid crystal 8OBA bent- dimer molecules is briefly discussed.

Supramolecular features of 2-(chlorophenyl)-3-[(chlorobenzylidene)-amino]-2,3-dihydroquinazolin-4(1H)-ones: A combined experimental and computational study

NASA Astrophysics Data System (ADS)

Mandal, Arkalekha; Patel, Bhisma K.

2018-03-01

The molecular structures of two isomeric 2-(chlorophenyl)-3-[(chlorobenzylidene)-amino] substituted 2,3-dihydroquinazolin-4(1H)-ones have been determined via single crystal XRD. Both isomers contain chloro substitutions on each of the phenyl rings and as a result a broad spectrum of halogen mediated weak interactions are viable in their crystal structures. The crystal packing of these compounds is stabilized by strong N-H⋯O hydrogen bond and various weak, non-classical hydrogen bonds acting synergistically. Both the molecules contain a chiral center and the weak interactions observed in them are either chiral self-discriminatory or chiral self-recognizing in nature. The weak interactions and spectral features of the compounds have been studied through experimental as well as computational methods including DFT, MEP, NBO and Hiresfeld surface analyses. In addition, the effect of different weak interactions to dictate either chiral self-recognition or self-discrimination in crystal packing has been elucidated.

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.

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.

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.

Concerted ligand exchange and the roles of counter anions in the reversible structural switching of crystalline peptide metallo-macrocycles.

PubMed

Miyake, Ryosuke; Shionoya, Mitsuhiko

2014-06-02

To understand reversible structural switching in crystalline materials, we studied the mechanism of reversible crystal-to-crystal transformation of a tetranuclear Ni(II) macrocycle consisting of artificial β-dipeptides. On the basis of detailed structural analyses and thermodynamic measurements made in a comparison of pseudo-isostructural crystals (NO3 and BF4 salts), we herein discuss how ligand-exchange reactions take place in the crystal due to changes in water content and temperature. Observations of the structural transformation of NO3 salt indicated that a pseudo crystalline phase transformation takes place through concerted ligand-exchange reactions at the four Ni(II) centers of the macrocycle with hydrogen bond switching. A mechanism for this ligand exchange was supported by IR spectroscopy. Thermodynamic measurements suggested that the favorable compensation relationship of the enthalpy changes due to water uptake and structural changes are keys to the reversible structural transformation. On the basis of a comparison with the pseudo-isostructural crystals, it is apparent that the crystal packing structure and the types of counter anions are important factors for facilitating reversible ligand exchange with single crystallinity.

Radiative Transfer and Satellite Remote Sensing of Cirrus Clouds Using FIRE-2-IFO Data

NASA Technical Reports Server (NTRS)

2000-01-01

Under the support of the NASA grant, we have developed a new geometric-optics model (GOM2) for the calculation of the single-scattering and polarization properties for arbitrarily oriented hexagonal ice crystals. From comparisons with the results computed by the finite difference time domain (FDTD) method, we show that the novel geometric-optics can be applied to the computation of the extinction cross section and single-scattering albedo for ice crystals with size parameters along the minimum dimension as small as approximately 6. We demonstrate that the present model converges to the conventional ray tracing method for large size parameters and produces single-scattering results close to those computed by the FDTD method for size parameters along the minimum dimension smaller than approximately 20. We demonstrate that neither the conventional geometric optics method nor the Lorenz-Mie theory can be used to approximate the scattering, absorption, and polarization features for hexagonal ice crystals with size parameters from approximately 5 to 20. On the satellite remote sensing algorithm development and validation, we have developed a numerical scheme to identify multilayer cirrus cloud systems using AVHRR data. We have applied this scheme to the satellite data collected over the FIRE-2-IFO area during nine overpasses within seven observation dates. Determination of the threshold values used in the detection scheme are based on statistical analyses of these satellite data.

Precise and accurate in situ Pb-Pb dating of apatite, monazite, and sphene by laser ablation multiple-collector ICP-MS

NASA Astrophysics Data System (ADS)

Willigers, B. J. A.; Baker, J. A.; Krogstad, E. J.; Peate, D. W.

2002-03-01

To evaluate in situ Pb dating by laser ablation multiple-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS), we analysed apatite, sphene, and monazite from Paleoproterozoic metamorphic rocks from West Greenland. Pb isotope ratios were also determined in the National Institute of Standards and Technology (NIST) 610 glass standard and were corrected for mass fractionation by reference to the measured thallium isotope ratio. The NIST 610 glass was used to monitor Pb isotope mass fractionation in the low Tl/Pb accessory minerals. Replicate analyses of the glass (1 to 2 min) yielded ratios with an external reproducibility comparable to conventional analyses of standard reference material 981 by thermal ionisation mass spectrometry (TIMS). Mineral grains were generally analysed with a 100-μm laser beam, although some monazite crystals were analysed at smaller spot sizes (10 and 25 μm). The common Pb isotope ratios required for age calculations were either measured on coexisting plagioclase by LA-MC-ICP-MS or could be ignored, as individual crystals exhibit sufficient Pb isotopic heterogeneity to perform isochron calculations on replicate analyses of single crystals. Mean mineral ages with the 204Pb ion beam measured in the multiplier were as follows: apatite, 1715 ± 23 m.y.; sphene, 1789 ± 11 m.y.; and monazite, 1783 to 1888 m.y., with relative uncertainties on individual monazite ages of <0.2% but highly reproducible age determinations on single monazite crystals (≪1%). Isochron ages calculated from several mineral analyses without assumption of common Pb also yield precise age determinations. Apatite and monazite Pb ages determined by in situ Pb isotope analysis are identical to those determined by conventional TIMS analysis of bulk mineral separates, and the analytical uncertainties of these short laser analyses with no prior mechanical or chemical separation are comparable to those obtained by TIMS. Detailed examination of the sphene in situ age data does, however, show a small discrepancy between the LA-MC-ICP-MS and TIMS ages (˜1% younger). High-resolution mass scans of the sphene during ablation clearly showed several small and as yet unidentified isobaric interferences that overlap with the 207Pb peak at the resolution conditions for measurement of isotope ratios. These might account for the age discrepancy between the LA-MC-ICP-MS and TIMS sphene ages. LA-MC-ICP-MS is a rapid, accurate, and precise method for in situ determination of Pb isotope ratios that can be used for geochronological studies in a manner similar to an ion microprobe, albeit currently at a somewhat degraded spatial resolution. Further modifications to the LA-MC-ICP-MS system, such as improved sensitivity, ion transmission, and LA methodology, may lead to this type of instrument becoming the method of choice for many types of in situ Pb isotope dating.

Crystal-field analysis of U3+ ions in K2LaX5 (X=Cl, Br or I) single crystals

NASA Astrophysics Data System (ADS)

Karbowiak, M.; Edelstein, N.; Gajek, Z.; Drożdżyński, J.

1998-11-01

An analysis of low temperature absorption spectra of U3+ ions doped in K2LaX5 (X=Cl, Br or I) single crystals is reported. The energy levels of the U3+ ion in the single crystals were assigned and fitted to a semiempirical Hamiltonian representing the combined atomic and crystal-field interactions at the Cs symmetry site. An analysis of the nephelauxetic effect and crystal-field splittings in the series of compounds is also reported.

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

Synthesis, structural, thermal and Hirshfeld surface analysis of novel [1,2,4]triazolo[3,4-b][1,3,4] thiadiazine carrying 1,4-benzothiazine-3-one moiety

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped single crystal of the title compound was grown by slow evaporation solution growth technique using ethanol as solvent. The grown single crystal was characterized using FT-IR, Single crystal XRD and Thermal analysis. The FT-IR spectrum confirms the molecular structure and identifies the different functional groups present in the compound. Single crystal XRD study reveals that the crystallized compound belongs to the monoclinic crystal system with P21/c space group and the corresponding cell parameters were identified. The thermal stability of the material was determined using both TGA and DTA analysis. The intermolecular interaction of each individual atom in the crystal lattice was estimated using Hirshfeld surface and finger print analysis.

Natural age dispersion arising from the analysis of broken crystals. Part I: Theoretical basis and implications for the apatite (U-Th)/He thermochronometer

NASA Astrophysics Data System (ADS)

Brown, Roderick W.; Beucher, Romain; Roper, Steven; Persano, Cristina; Stuart, Fin; Fitzgerald, Paul

2013-12-01

Over the last decade major progress has been made in developing both the theoretical and practical aspects of apatite (U-Th)/He thermochronometry and it is now standard practice, and generally seen as best practice, to analyse single grain aliquots. These individual prismatic crystals are often broken and are fragments of larger crystals that have broken during mineral separation along the weak basal cleavage in apatite. This is clearly indicated by the common occurrence of only 1 or no clear crystal terminations present on separated apatite grains, and evidence of freshly broken ends when grains are viewed using a scanning electron microscope. This matters because if the 4He distribution within the whole grain is not homogeneous, because of partial loss due to thermal diffusion for example, then the fragments will all yield ages different from each other and from the whole grain age. Here we use a numerical model with a finite cylinder geometry to approximate 4He ingrowth and thermal diffusion within hexagonal prismatic apatite crystals. This is used to quantify the amount and patterns of inherent, natural age dispersion that arises from analysing broken crystals. A series of systematic numerical experiments were conducted to explore and quantify the pattern and behaviour of this source of dispersion using a set of 5 simple thermal histories that represent a range of plausible geological scenarios. In addition some more complex numerical experiments were run to investigate the pattern and behaviour of grain dispersion seen in several real data sets. The results indicate that natural dispersion of a set of single fragment ages (defined as the range divided by the mean) arising from fragmentation alone varies from c. 7% even for rapid (c. 10 °C/Ma), monotonic cooling to over 50% for protracted, complex histories that cause significant diffusional loss of 4He. The magnitude of dispersion arising from fragmentation scales with the grain cylindrical radius, and is of a similar magnitude to dispersion expected from differences in absolute grain size alone (spherical equivalent radii of 40-150 μm). This source of dispersion is significant compared with typical analytical uncertainties on individual grain analyses (c. 6%) and standard deviations on multiple grain analyses from a single sample (c. 10-20%). Where there is a significant difference in the U and Th concentration of individual grains (eU), the effect of radiation damage accumulation on 4He diffusivity (assessed using the RDAAM model of Flowers et al. (2009)) is the primary cause of dispersion for samples that have experienced a protracted thermal history, and can cause dispersion in excess of 100% for realistic ranges of eU concentration (i.e. 5-100 ppm). Expected natural dispersion arising from the combined effects of reasonable variations in grain size (radii 40-125 μm), eU concentration (5-150 ppm) and fragmentation would typically exceed 100% for complex thermal histories. In addition to adding a significant component of natural dispersion to analyses, the effect of fragmentation also acts to decouple and corrupt expected correlations between grain ages and absolute grain size and to a lesser extent between grain age and effective uranium concentration (eU). Considering fragmentation explicitly as a source of dispersion and analysing how the different sources of natural dispersion all interact with each other provides a quantitative framework for understanding patterns of dispersion that otherwise appear chaotic. An important outcome of these numerical experiments is that they demonstrate that the pattern of age dispersion arising from fragmentation mimics the pattern of 4He distribution within the whole grains, thus providing an important source of information about the thermal history of the sample. We suggest that if the primary focus of a study is to extract the thermal history information from (U-Th)/He analyses then sampling and analytical strategies should aim to maximise the natural dispersion of grain ages, not minimise it, and should aim to analyse circa 20-30 grains from each sample. The key observations and conclusions drawn here are directly applicable to other thermochronometers, such as the apatite, rutile and titanite U-Pb systems, where the diffusion domain is approximated by the physical grain size.

Crystal structure, molecular docking, and biological activity of the zinc complexes with 2-thenoyltrifluoroacetone and N-donor heterocyclic ligands

NASA Astrophysics Data System (ADS)

Eshaghi Malekshah, Rahime; Salehi, Mehdi; Kubicki, Maciej; Khaleghian, Ali

2017-12-01

Two novel mononuclear complexes, [Zn (TTA) (bipy)Cl] (1) and [Zn (TTA) (phen)Cl] (2) (TTA = 4,4,4-Trifluoro-1-(2-furyl)-1,3-butanedione, phen = 1,10-phenanthroline and bipy 2, 2ʹ-bipyridine), were synthesized and fully characterized by elemental analyses, 1H NMR, UV-Vis, FTIR spectroscopy, and conductivity measurements. The crystal structures of these two mono-nuclear zinc (II) complexes were determined by X-ray single-crystal diffraction. The result of X-ray diffraction analyses revealed that both complexes have distorted tetragonal-pyramid structures. In MTT cytotoxicity studies, these Zn (II) complexes exhibited antitumor activity against MCF-7 and MKN-45 cell lines. It was also found that the proliferation rate of MCF-7 and MKN-45 cells decreased after treatment with the above-mentioned complexes. In addition, the apoptosis-inducing activity was assessed by AO/EB (Acridine Orange/Ethidium bromide) staining assay and found that they have the potential to act as effective metal-based anticancer drugs. Finally, the molecular docking studies showed that complex 2 strongly binds through minor groove with DNA by relative binding energy -7.33 kcal mol-1.

On capturing the grain-scale elastic and plastic anisotropy of alpha-Ti with spherical nanoindentation and electron back-scattered diffraction

DOE PAGES

Weaver, Jordan S.; Priddy, Matthew W.; McDowell, David L.; ...

2016-09-01

Here, spherical nanoindentation combined with electron back-scattered diffraction has been employed to characterize the grain-scale elastic and plastic anisotropy of single crystal alpha-Ti of two different compositions (in two different titanium alloys). Data analyses protocols needed to reliably extract the desired properties of interest are extended and demonstrated in this paper. Specifically, the grain-scale mechanical response is extracted in the form of indentation stress-strain curves for commercially pure (CP-Ti) alpha-Ti and alloyed (Ti-64) titanium from measurements on polycrystalline samples. The results are compared with responses of single crystals and nanoindentation tests (hardness and modulus) from the literature, and the measuredmore » indentation moduli are validated using crystal-elastic finite element simulations. The results obtained in this study show that (i) it is possible to characterize reliably the elastic and plastic anisotropy of alpha-Ti (hcp) of varying alloying contents with spherical nanoindentation stress-strain curves, (ii) the indentation modulus of alpha-Ti-64 is 5–10% less than CP-Ti, and (iii) the indentation yield strength of alpha-Ti-64 is 50–80% higher than CP-Ti.« less

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.

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.

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.

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR

NASA Astrophysics Data System (ADS)

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-01

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO4·KOH·H2O or more accurately as KCd2(CrO4)2(H3O2) illustrating the μ-H3O2- species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V).

Characterisation of the rare cadmium chromate pigment in a 19th century tube colour by Raman, FTIR, X-ray and EPR.

PubMed

Christiansen, Marie Bitsch; Sørensen, Mikkel Agerbæk; Sanyova, Jana; Bendix, Jesper; Simonsen, Kim Pilkjær

2017-03-15

In an investigation of the artists' materials used by P. S. Krøyer the contents of the tube colours found in Krøyer's painting cabinet were examined. In most cases, the results of the pigment analyses were as expected based on our knowledge of artists' colours used in the late 1800s and early 1900s. However, in one of the tube colours labelled "Jaune de Cadmium Citron" (cadmium lemon yellow) an extremely rare cadmium chromate pigment was found. The pigment was analysed and characterised by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), powder X-ray diffraction (PXRD), single-crystal X-ray crystallography, and electron paramagnetic resonance (EPR) spectroscopy. Cadmium chromate was synthesised by precipitation from an aqueous solution of cadmium nitrate and potassium chromate, and the resulting yellow crystals proved identical to the pigment found in the tube colour "Jaune de Cadmium Citron". The structure determined by single-crystal X-ray diffraction identified the pigment as 2CdCrO 4 ·KOH·H 2 O or more accurately as KCd 2 (CrO 4 ) 2 (H 3 O 2 ) illustrating the μ-H 3 O 2 - species. The yellow colour of the paint sample taken from the tube had a greenish hue, which became even more prominent upon storage and drying. EPR analysis of the sample showed the presence of paramagnetic degradation products containing Cr(III) and Cr(V). Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Synthesis, crystal structure investigation, spectroscopic characterizations and DFT computations on a novel 1-(2-chloro-4-phenylquinolin-3-yl)ethanone

NASA Astrophysics Data System (ADS)

Murugavel, S.; Stephen, C. S. Jacob Prasanna; Subashini, R.; Reddy, H. Raveendranatha; AnanthaKrishnan, Dhanabalan

2016-10-01

The title compound 1-(2-chloro-4-phenylquinolin-3-yl)ethanone (CPQE) was synthesised effectively by chlorination of 3-acetyl-4-phenylquinolin-2(1H)-one (APQ) using POCl3 reagent. Structural and vibrational spectroscopic studies were performed by utilizing single crystal X-ray diffraction, FTIR and NMR spectral analysis along with DFT method utilizing GAUSSIAN‧ 03 software. Veda program has been employed to perform a detailed interpretation of vibrational spectra. Mulliken population analyses on atomic charges, MEP, HOMO-LUMO, NBO, Global chemical reactivity descriptors and thermodynamic properties have been examined by (DFT/B3LYP) method with the 6-311G(d,p) basis set level.

Influence of other rare earth ions on the optical refrigeration efficiency in Yb:YLF crystals.

PubMed

Di Lieto, Alberto; Sottile, Alberto; Volpi, Azzurra; Zhang, Zhonghan; Seletskiy, Denis V; Tonelli, Mauro

2014-11-17

We investigated the effect of rare earth impurities on the cooling efficiency of Yb³⁺:LiYF₄ (Yb:YLF). The refrigeration performance of two single crystals, doped with 5%-at. Yb and with identical history but with different amount of contaminations, have been compared by measuring the cooling efficiency curves. Spectroscopic and elemental analyses of the samples have been carried out to identify the contaminants, to quantify their concentrations and to understand their effect on the cooling efficiencies. A model of energy transfer processes between Yb and other rare earth ions is suggested, identifying Erbium and Holmium as elements that produce a detrimental effect on the cooling performance.

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.

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.

Room temperature aluminum antimonide radiation detector and methods thereof

DOEpatents

Lordi, Vincenzo; Wu, Kuang Jen J.; Aberg, Daniel; Erhart, Paul; Coombs, III, Arthur W; Sturm, Benjamin W

2015-03-03

In one embodiment, a method for producing a high-purity single crystal of aluminum antimonide (AlSb) includes providing a growing environment with which to grow a crystal, growing a single crystal of AlSb in the growing environment which comprises hydrogen (H.sub.2) gas to reduce oxide formation and subsequent incorporation of oxygen impurities in the crystal, and adding a controlled amount of at least one impurity to the growing environment to effectively incorporate at least one dopant into the crystal. In another embodiment, a high energy radiation detector includes a single high-purity crystal of AlSb, a supporting structure for the crystal, and logic for interpreting signals obtained from the crystal which is operable as a radiation detector at a temperature of about 25.degree. C. In one embodiment, a high-purity single crystal of AlSb includes AlSb and at least one dopant selected from a group consisting of selenium (Se), tellurium (Te), and tin (Sn).

Implications of Bishop Tuff zircon U-Pb ages for rates of zircon growth and magma accumulation

NASA Astrophysics Data System (ADS)

Reid, M. R.; Schmitt, A. K.

2012-12-01

Rates of geologic processes obtained from natural studies rely on accurate geochronologic information. An important benchmark in geochronology as well as a valuable source of insights into the evolution of voluminous explosive eruptions is the >600 km3 Bishop Tuff (BT). A recently determined weighted mean 206Pb/238U date of 767.1±0.9 ka for a BT zircon population [1] is indistinguishable from the recalibrated 40Ar/39Ar sanidine date of 767.4±2.2 ka [2], potentially providing a key intercalibration point between astronomical and radio-isotopic dating approaches. Consequences of these results are linear zircon growth rates of >1×10-14 cm/sec and magma accumulation rates of >200 km3/ka. In contrast, spatially selective SIMS U-Pb dating of BT zircons yielded mean pre-eruption ages of 850 ka [3], a difference that raises questions about the validity of intercalibration between U-Pb and K-Ar dating methods and the history of magma accumulation. We obtained new SIMS analyses of the BT zircons using more spatially and analytically sensitive methods and verifying our accuracy against the TIMS dated Quaternary zircon 61.308A (2.488±0.002 Ma). Analyses were performed on zircon rims and on oriented cross-sections exposed during optical interferometry-calibrated serial sectioning removing the outermost ~31 μm. Sputtering by a 100 nA ion beam versus the normally employed 10-12 nA beam resulted in enhanced radiogenic Pb yields and analytical uncertainties for Quaternary zircon approaching the U-Pb age reproducibility of the primary zircon standard (~1-2 % for AS3). Ages obtained at ~31 μm depth (representing <5% of crystal growth in most cases) average 892±26ka (MSWD=0.29), corroborating previous evidence for residence times of several tens of ka. Rim ages average 781±22 ka (MSWD=0.61), overlapping Ar/Ar determinations of eruption age and corroborating the importance of near-eruption aged zircon growth. Our results confirm the presence of BT zircon domains that predate eruption by tens of ka, domains that could be difficult to detect by single crystal analyses. SIMS analyses can selectively sample more interior portions of grains whereas whole grain TIMS analyses will be volumetrically biased towards the outermost ~20% of the BT zircons. Spots centered on BT zircon cores sample a domain representing only a few volume percent of the crystal; if mantled completely by eruption-aged growth, single crystal zircon ages are predicted to be <5 ka older than eruption, extrapolating from the SIMS dates. When, compared to grain interiors, the greater average near-rim U concentrations are factored into this mass balance, the influence of these older domains is further diminished. A scenario that can at least partially reconcile the disparate zircon dates in the context of evolution of the BT and the dynamics of zircon crystallization is as follows: (1) zircon nucleation and relatively rapid growth an average of ~100 ka before eruption; (2) significant decay in zircon growth rates as temperatures and Zr melt gradients relax; and, finally, (3) mantling of earlier zircon cores by rejuvenation and renewed BT zircon growth during the lead-up to eruption. Comparisons between spot and single grain dating show that most zircon growth likely occurred close to eruption. [1] Crowley et al., 2007.Geology 35, 1123. [2] Rivera et al., 2011. Earth Planet. Sci. Lett. 311, 420. [3] Simon and Reid, 2005. Earth Planet. Sci. Lett. 235, 123.

Low Leakage Superconducting Tunnel Junctions with a Single Crystal Al2O3 Barrier

DTIC Science & Technology

2016-03-30

have recently implemented Josephson junction superconducting devices into qubits [1-6]. Before a multi -qubit quantum computer is realized, however...Low-Leakage Superconducting Tunnel Junctions with a Single-Crystal Al2O3 Barrier* S Oh1,2, K Cicak1, R McDermott3, K B Cooper3, K D Osborn1, R W...growth scheme for single-crystal Al2O3 tunnel barriers. The barriers are epitaxially grown on single-crystal rhenium (Re) base electrodes that are

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, R. F.; Burger, A.; Dudley, M.; Matyi, R.; Ramachandran, N.; Sha, Yi-Gao; Volz, M.; Shih, Hung-Dah

1999-01-01

Complete and systematic ground-based experimental and theoretical analyses on the Physical Vapor Transport (PVT) of ZnSe and related ternary compound semiconductors have been performed. The analyses included thermodynamics, mass flux, heat treatment of starting material, crystal growth, partial pressure measurements, optical interferometry, chemical analyses, photoluminescence, microscopy, x-ray diffraction and topography as well as theoretical, analytical and numerical analyses. The experimental results showed the influence of gravity orientation on the characteristics of: (1) the morphology of the as-grown crystals as well as the as-grown surface morphology of ZnSe and Cr doped ZnSe crystals; (2) the distribution of impurities and defects in ZnSe grown crystals; and (3) the axial segregation in ZnSeTe grown crystals.

Cyanide-bridged decanuclear cobalt-iron cage.

PubMed

Shiga, Takuya; Tetsuka, Tamaki; Sakai, Kanae; Sekine, Yoshihiro; Nihei, Masayuki; Newton, Graham N; Oshio, Hiroki

2014-06-16

A cyanide-bridged decanuclear [Co6Fe4] cluster was synthesized by a one-pot reaction, and the magnetic properties and electronic configuration were investigated. The complex displayed thermally controlled electron-transfer-coupled spin transition (ETCST) behavior between Co(III) low-spin-NC-Fe(II) low-spin and Co(II) high-spin-NC-Fe(III) low-spin states, as confirmed by single-crystal X-ray, magnetic, and Mössbauer analyses.

Photoluminescent lead(II) coordination polymers stabilised by bifunctional organoarsonate ligands

NASA Astrophysics Data System (ADS)

Lin, Jian-Di; Onet, Camelia I.; Schmitt, Wolfgang

2015-04-01

Four lead(II) coordination polymers were isolated under hydro(solvo)thermal conditions. The applied synthetic methodology takes advantage of the coordination behaviour of a new bifunctional organoarsonate ligand, 4-(1, 2, 4-triazol-4-yl)phenylarsonic acid (H2TPAA) and involves the variation of lead(II) reactants, metal/ligand mole ratios, and solvents. The constitutional composition of the four lead(II) coordination polymers can be formulated as [Pb2(TPAA)(HTPAA)(NO3)]·6H2O (1), [Pb2(TPAA)(HTPAA)2]·DMF·0.5H2O (DMF = N, N-Dimethylformamide) (2), [Pb2Cl2(TPAA)H2O] (3), and [Pb3Cl(TPAA)(HTPAA)2H2O]Cl (4). The compounds were characterized by single-crystal and powder x-ray diffraction techniques, thermogravimetric analyses, infra-red spectroscopy, and elemental analyses. Single-crystal x-ray diffraction reveals that 1 and 2 represent two-dimensional (2D) layered structures whilst 3 and 4 form three-dimensional (3D) frameworks. The structures of 1, 2, and 4 contain one-dimensional (1D) {PbII/AsO3} substructures, while 3 is composed of 2D {PbII/AsO3} arrays. Besides their interesting topologies, 1-4 all exhibit photoluminescence properties in the solid state at room temperature.

On the nature of the reversibility of hydration-dehydration on the crystal structure and magnetism of the ferrimagnet [MnII(enH)(H2O)][CrIII(CN)6].H2O.

PubMed

Yoshida, Yusuke; Inoue, Katsuya; Kurmoo, Mohamedally

2009-01-05

We report the synthesis, crystal structure, and thermal and magnetic properties of the two-dimensional achiral soft ferrimagnet [Mn(II)(enH)(H(2)O)][Cr(III)(CN)(6)].H(2)O (1), en = 1,2-diaminoethane, as well as the recyclability of the dehydration and rehydration and their influence on the crystal structure and its magnetic properties. Unlike [Mn(S-pnH)(H(2)O)][Cr(CN)(6)].H(2)O (2S, pn = 1,2-diaminopropane), which is a chiral (P2(1)2(1)2(1)) enantiopure ferrimagnet (T(C) = 38 K), 1 crystallizes in the achiral orthorhombic Pcmn space group, having a similar two-dimensional square network of Mn-Cr with bridging cyanide, and 1 behaves also as a soft ferrimagnet (T(C) = 42 K). X-ray diffraction experiments on a single crystal of 1 indicate a transformation from a single crystal to an amorphous phase upon dehydrataion and partial recovery of its crystallinity upon rehydration. The dehydrated phase 1-DP exhibits long-range ordering at 75 K to a ferrimagnetic state and coercive field at 2 K of 100 Oe, which are a higher critical temperature and coercive field than for the virgin sample (H(C) = 60 Oe). Thermogravimetric analyses indicate that the crystallinity deteriorates upon hydration-dehydration cycling, with persistence toward the amorphous phase, as also seen by magnetization measurements. This effect is associated with an increase of statistical disorder inherent in the dehydration-rehydration process. X-ray powder diffraction suggests that 1-DP may retain order within the layers but loses coherence in the stacking of the layers.

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.

Attenuation of thermal neutrons by an imperfect single crystal

NASA Astrophysics Data System (ADS)

Naguib, K.; Adib, M.

1996-06-01

A semi-empirical formula is given which allows one to calculate the total thermal cross section of an imperfect single crystal as a function of crystal constants, temperature and neutron energy E, in the energy range between 3 meV and 10 eV. The formula also includes the contribution of the parasitic Bragg scattering to the total cross section that takes into account the crystal mosaic spread value and its orientation with respect to the neutron beam direction. A computer program (ISCANF) was developed to calculate the total attenuation of neutrons using the proposed formula. The ISCANF program was applied to investigate the neutron attenuation through a copper single crystal. The calculated values of the neutron transmission through the imperfect copper single crystal were fitted to the measured ones in the energy range 3 - 40 meV at different crystal orientations. The result of fitting shows that use of the computer program ISCANF allows one to predict the behaviour of the total cross section of an imperfect copper single crystal for the whole energy range.

Seeded growth of boron arsenide single crystals with high thermal conductivity

NASA Astrophysics Data System (ADS)

Tian, Fei; Song, Bai; Lv, Bing; Sun, Jingying; Huyan, Shuyuan; Wu, Qi; Mao, Jun; Ni, Yizhou; Ding, Zhiwei; Huberman, Samuel; Liu, Te-Huan; Chen, Gang; Chen, Shuo; Chu, Ching-Wu; Ren, Zhifeng

2018-01-01

Materials with high thermal conductivities are crucial to effectively cooling high-power-density electronic and optoelectronic devices. Recently, zinc-blende boron arsenide (BAs) has been predicted to have a very high thermal conductivity of over 2000 W m-1 K-1 at room temperature by first-principles calculations, rendering it a close competitor for diamond which holds the highest thermal conductivity among bulk materials. Experimental demonstration, however, has proved extremely challenging, especially in the preparation of large high quality single crystals. Although BAs crystals have been previously grown by chemical vapor transport (CVT), the growth process relies on spontaneous nucleation and results in small crystals with multiple grains and various defects. Here, we report a controllable CVT synthesis of large single BAs crystals (400-600 μm) by using carefully selected tiny BAs single crystals as seeds. We have obtained BAs single crystals with a thermal conductivity of 351 ± 21 W m-1 K-1 at room temperature, which is almost twice as conductive as previously reported BAs crystals. Further improvement along this direction is very likely.

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

Ji, Xiaoyu; Lei, Shiming; Yu, Shih -Ying

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

Mid-IR supercontinuum generation and applications: a review

NASA Astrophysics Data System (ADS)

Yin, Shizhuo; Ruffin, Paul; Brantley, Christina; Edwards, Eugene; Luo, Claire

2014-09-01

In this paper, a review on mid-IR supercontinuum generation (SCG) and its applications is presented. First, the physical mechanism of the supercontinuum generation in IR crystal fiber is introduced. Second, the recent progress on IR single crystal fiber, in particular ultrathin core double cladding IR single crystal fiber is described. Third, the transmission characteristics of mid-IR crystal fiber is illustrated. Fourth, the mid-IR supercontinuum generation in IR single crystal fiber is presented. Finally, the application of IR supercontinuum for smart target recognition is illustrated

Size dependence of nanoscale wear of silicon carbide

Treesearch

Chaiyapat Tangpatjaroen; David Grierson; Steve Shannon; Joseph E. Jakes; Izabela Szlufarska

2017-01-01

Nanoscale, single-asperity wear of single-crystal silicon carbide (sc- SiC) and nanocrystalline silicon carbide (nc-SiC) is investigated using single-crystal diamond nanoindenter tips and nanocrystalline diamond atomic force microscopy (AFM) tips under dry conditions, and the wear behavior is compared to that of single-crystal silicon with both thin and thick native...

Anisotropic Laminar Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

2006-01-01

The design, fabrication, and testing of a flexible, laminar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d33 piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d33 estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

Anisotropic Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

2004-01-01

The design, fabrication, and testing of a flexible, planar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d(sub 33) piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d(sub 33) estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

Three-Dimensional Conformation of Folded Polymers in Single Crystals

NASA Astrophysics Data System (ADS)

Hong, You-lee; Yuan, Shichen; Li, Zhen; Ke, Yutian; Nozaki, Koji; Miyoshi, Toshikazu

2015-10-01

The chain-folding mechanism and structure of semicrystalline polymers have long been controversial. Solid-state NMR was applied to determine the chain trajectory of 13C CH3 -labeled isotactic poly(1-butene) (i PB 1 ) in form III chiral single crystals blended with nonlabeled i PB 1 crystallized in dilute solutions under low supercooling. An advanced 13C - 13C double-quantum NMR technique probing the spatial proximity pattern of labeled 13C nuclei revealed that the chains adopt a three-dimensional (3D) conformation in single crystals. The determined results indicate a two-step crystallization process of (i) cluster formation via self-folding in the precrystallization stage and (ii) deposition of the nanoclusters as a building block at the growth front in single crystals.

High-pressure floating-zone growth of perovskite nickelate LaNiO 3 single crystals

DOE PAGES

Zhang, Junjie; Zheng, Hong; Ren, Yang; ...

2017-04-07

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

Solution-processed, Self-organized Organic Single Crystal Arrays with Controlled Crystal Orientation

PubMed Central

Kumatani, Akichika; Liu, Chuan; Li, Yun; Darmawan, Peter; Takimiya, Kazuo; Minari, Takeo; Tsukagoshi, Kazuhito

2012-01-01

A facile solution process for the fabrication of organic single crystal semiconductor devices which meets the demand for low-cost and large-area fabrication of high performance electronic devices is demonstrated. In this paper, we develop a bottom-up method which enables direct formation of organic semiconductor single crystals at selected locations with desired orientations. Here oriented growth of one-dimensional organic crystals is achieved by using self-assembly of organic molecules as the driving force to align these crystals in patterned regions. Based upon the self-organized organic single crystals, we fabricate organic field effect transistor arrays which exhibit an average field-effect mobility of 1.1 cm2V−1s−1. This method can be carried out under ambient atmosphere at room temperature, thus particularly promising for production of future plastic electronics. PMID:22563523

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.

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.

Synthesis, crystal structure, NLO and Hirshfeld surface analysis of 1,2,3-triazolyl chalcone single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped brown coloured single crystal of the title compound was grown by slow evaporation technique using methanol as solvent. The grown crystal was characterized using FT-IR, Single crystal XRD, UV-visible and NLO studies. Crystal structure was confirmed by FT-IR study and the functional groups were identified. XRD study reveals that the crystal belongs to orthorhombic crystal system with pnaa space group and the corresponding cell parameters were calculated. UV-visible spectrum shows that the crystal is transparent in the entire visible region and absorption takes place in the UV-range. NLO efficiency of the crystal obtained 0.66 times that of urea was determined by SHG test. The intermolecular interaction and percentage contribution of each individual atom in the crystal lattice was quantized using Hirshfeld surface and 2D finger print analysis.

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 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).

Asymmetric flavone-based liquid crystals: synthesis and properties

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

Timmons, Daren J.; Jordan, Abraham J.; Kirchon, Angelo A.

2017-02-01

A series of flavones (n-F) substituted at the 4', and 6 positions was prepared, characterised by NMR (1H,13C), HRMS, and studied for liquid crystal properties. The 4'-alkoxy,6-methoxyflavones (4-F–16-F) exhibit varying ranges of nematic and smectic A phases as evidenced by polarised optical microscopy and differential scanning calorimetry (DSC). As the tail length is increased, the smectic phase becomes more prevalent. Smectic phases for (8-F–16-F) were further analysed by powder X-ray diffraction (XRD), and the rate of structural transformations was explored by combined DSC/XRD studies. Flavonol 6-F–OH was also prepared but no mesogenic behaviour was observed. The molecular structures of 6-Fmore » and 6-F–OH were determined by single-crystal XRD and help to explain the differences in material properties. Additionally, fluorescence and electrochemical studies were conducted on solutions of n-F.« less

Structure determination and characterization of two rare-earth molybdenum borate compounds: LnMoBO(6) (Ln = La, Ce).

PubMed

Zhao, Dan; Cheng, Wen-Dan; Zhang, Hao; Hang, Shu-Ping; Fang, Ming

2008-07-28

The structural, optical, and electronic properties of two rare-earth molybdenum borate compounds, LnMoBO(6) (Ln = La, Ce), have been investigated by means of single-crystal X-ray diffraction, elemental analyses, and spectral measurements, as well as calculations of energy band structures, density of states, and optical response functions by the density functional method. The title compounds, which crystallize in monoclinic space group P2(1)/c, possess a similar network of interconnected [Ce(2)(MoO(4))(2)](2+) chains and [BO(2)](-) wavy chains. Novel 1D molybdenum oxide chains are contained in their three-dimensional (3D) networks. The calculated results of crystal energy band structure by the density functional theory (DFT) method show that the solid-state compound LaMoBO(6) is a semiconductor with indirect band gaps.

A new series of lanthanide coordination polymers with 2,2‧-bipyridine and glutaric acid: Synthesis, crystal structures and properties of [Ln(bipy)(glut)(NO3)

NASA Astrophysics Data System (ADS)

Wang, Chunguang; Xing, Yongheng; Li, Zhangpeng; Li, Jing; Zeng, Xiaoqing; Ge, Maofa; Niu, Shuyun

2009-08-01

A series of new lanthanide coordination polymers, with the formula [Ln(bipy)(glut)(NO 3)] (Ln = Eu ( 1), Tb ( 2), Sm ( 3), Pr ( 4); bipy = 2,2'-bipyridine; H 2glut = glutaric acid), have been synthesized under the hydrothermal condition and characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction. Structural analyses reveal that all four complexes are isostructural and crystallized in monoclinic system, P2 1/ c space group. For these complexes, the Ln 3+ are all linked through glutaric acid ligands to form 1D chain-like polymeric structures, and bipy and NO3- are coordinated on two sides of the chains. The thermogravimetric analysis of 1 and photoluminescent properties of 1 and 2 are discussed in detail.

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.

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.

A STUDY OF DISLOCATION STRUCTURE OF SUBBOUNDARIES IN MOLYBDENUM SINGLE CRYSTALS,

DTIC Science & Technology

MOLYBDENUM, *DISLOCATIONS), GRAIN STRUCTURES(METALLURGY), SINGLE CRYSTALS, ZONE MELTING, ELECTRON BEAM MELTING, GRAIN BOUNDARIES, MATHEMATICAL ANALYSIS, ETCHED CRYSTALS, ETCHING, ELECTROEROSIVE MACHINING, CHINA

Growth of single crystals from solutions using semi-permeable membranes

NASA Astrophysics Data System (ADS)

Varkey, A. J.; Okeke, C. E.

1983-05-01

A technique suitable for growth of single crystals from solutions using semi-preamble membranes is described. Using this technique single crystals of copper sulphate, potassium bromide and ammonium dihydrogen phosphate have been successfully grown. Advantages of this technique over other methods are discussed.

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.

Effects of Ca/Sr ratio control on optical and scintillation properties of Eu-doped Li(Ca,Sr)AlF6 single crystals

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Tanaka, Chieko; Kurosawa, Shunsuke; Yamaji, Akihiro; Ohashi, Yuji; Kamada, Kei; Nikl, Martin; Yoshikawa, Akira

2018-05-01

Eu-doped Li(Ca,Sr)AlF6 [Eu:LiCSAF] single crystals with various Ca/Sr ratios were grown by the micro-pulling-down method, and their optical and scintillation properties were investigated to reveal the effects of Ca/Sr ratio on optical and scintillation properties of the Eu:LiCSAF single crystals. The Li(Ca1-x-ySrxEuy)AlF6 single crystals could be grown in 0 ≤ x ≤ 0.1, 0.5 ≤ x ≤ 1.0 and y = 0.02 while the Eu:LiCSAF crystals with x = 0.2, 0.25 and 0.4 included two colquiriite-type phases with different lattice parameters. The Li(Ca1-x-ySrxEuy)AlF6 single crystal with x = 0.25 and y = 0.02 showed the highest light yield under neutron irradiation.

Highly reproducible alkali metal doping system for organic crystals through enhanced diffusion of alkali metal by secondary thermal activation.

PubMed

Lee, Jinho; Park, Chibeom; Song, Intek; Koo, Jin Young; Yoon, Taekyung; Kim, Jun Sung; Choi, Hee Cheul

2018-05-16

In this paper, we report an efficient alkali metal doping system for organic single crystals. Our system employs an enhanced diffusion method for the introduction of alkali metal into organic single crystals by controlling the sample temperature to induce secondary thermal activation. Using this system, we achieved intercalation of potassium into picene single crystals with closed packed crystal structures. Using optical microscopy and Raman spectroscopy, we confirmed that the resulting samples were uniformly doped and became K 2 picene single crystal, while only parts of the crystal are doped and transformed into K 2 picene without secondary thermal activation. Moreover, using a customized electrical measurement system, the insulator-to-semiconductor transition of picene single crystals upon doping was confirmed by in situ electrical conductivity and ex situ temperature-dependent resistivity measurements. X-ray diffraction studies showed that potassium atoms were intercalated between molecular layers of picene, and doped samples did not show any KH- nor KOH-related peaks, indicating that picene molecules are retained without structural decomposition. During recent decades, tremendous efforts have been exerted to develop high-performance organic semiconductors and superconductors, whereas as little attention has been devoted to doped organic crystals. Our method will enable efficient alkali metal doping of organic crystals and will be a resource for future systematic studies on the electrical property changes of these organic crystals upon doping.

Fe-Al alloy single-crystal thin film preparation for basic magnetic measurements

NASA Astrophysics Data System (ADS)

Abe, Tatsuya; Kawai, Tetsuroh; Futamoto, Masaaki; Ohtake, Mitsuru; Inaba, Nobuyuki

2018-04-01

Fe100-xAlx (x = 0, 4, 10, 20, 30 at. %) alloy films of 40 nm thickness are prepared on MgO(001) single-crystal substrates by varying substrate temperature from room temperature to 600 °C. Single-crystal films of (001) orientation with bcc-based disordered A2 structure are obtained for the Al content range of x = 0 - 20 at. %. An ordered phase of DO3 structure is observed in Fe70Al30 films prepared at temperatures higher than 200 °C, whereas (001) oriented single-crystal films of A2 structure are obtained when prepared at room temperature. The film surface profile does not depend much on the film composition, while the surface roughness increases with increasing substrate temperature. Island-like crystals are observed for films prepared at 600°C for all compositions. Difference in lattice spacing measured parallel and perpendicular to the substrate is noted for the single-crystal thin films and it increases with increasing Al content. The lattice strain in single-crystal film is caused possibly to accommodate the lattice mismatch with the MgO substrate. The (001)-oriented single-crystal films with A2 structure show four-fold symmetries in in-plane magnetic anisotropy with the easy magnetization axis A2[100] and the hard magnetization axis A2[110], whereas the films with DO3 ordered structure show almost isotropic magnetic properties.

Advanced Czochralski silicon growth technology for photovoltaic modules

NASA Technical Reports Server (NTRS)

Daud, T.; Kachare, A. H.

1982-01-01

Several economic analyses had indicated that large-diameter, multiple ingot growth using a single crucible with melt replenishment would be required for Cz growth to be economically viable. Based on the results of these analyses, two liquid and two solid feed melt replenishment approaches were initiated. The sequential solid feed melt replenishment approach, which demonstrated elements of technical feasibility is described in detail in this paper. Growth results of multiple ingots (10-cm-diameter, totaling 100 kg; and 15-cm-diameter, totaling 150 kg weight per crucible) are presented. Solar cells were fabricated and analyzed to evaluate the effects of structure and chemical purities as a result of multiple growth. The results indicate that, with semiconductor-grade silicon, feedstock impurity build-up does not seem to degrade cell performance. For polycrystalline cells, the average efficiencies are 15 to 25% lower than those of single crystalline cells. Concerns regarding single crystal yields, crucible quality and growth speed are indicated, and present status and future research thrusts are also discussed.

Temperature dependence of single-crystal elastic constants of flux-grown alpha-GaPO(4).

PubMed

Armand, P; Beaurain, M; Rufflé, B; Menaert, B; Papet, P

2009-06-01

The lattice parameter change with respect to temperature (T) has been measured using high-temperature powder X-ray diffraction techniques for high-temperature flux-grown GaPO(4) single crystals with the alpha-quartz structure. The lattice and the volume linear thermal expansion coefficients in the temperature range 303-1173 K were computed from the X-ray data. The percentage linear thermal expansions along the a and c axes at 1173 K are 1.5 and 0.51, respectively. The temperature dependence of the mass density rho of flux-grown GaPO(4) single crystals was evaluated using the volume thermal expansion coefficient alpha(V)(T) = 3.291 x 10(-5) - 2.786 x 10(-8) [T] + 4.598 x 10(-11)[T](2). Single-crystal high-resolution Brillouin spectroscopy measurements have been carried out at ambient pressure from 303 to 1123 K to determine the elastic constants C(IJ) of high-temperature flux-grown GaPO(4) material. The single-crystal elastic moduli were calculated using the sound velocities via the measured Brillouin frequency shifts Deltanu(B). These are, to our knowledge, the highest temperatures at which single-crystal elastic constants of alpha-GaPO(4) have been measured. Most of the room-temperature elastic constant values measured on flux-grown GaPO(4) material are higher than the ones found for hydrothermally grown GaPO(4) single crystals. The fourth-order temperature coefficients of both the Brillouin frequency shifts T(nuB)((n)) and the single-crystal elastic moduli T(C(IJ))((n)) were obtained. The first-order temperature coefficients of the C(IJ) are in excellent agreement with previous reports on low-temperature hydrothermally grown alpha-GaPO(4) single crystals, while small discrepancies in the higher-order temperature coefficients are observed. This is explained in terms of the OH content in the GaPO(4) network, which is an important parameter in the crystal thermal behavior.

Structure and Growth Control of Organic–Inorganic Halide Perovskites for Optoelectronics: From Polycrystalline Films to Single Crystals

PubMed Central

Chen, Yani; He, Minhong; Peng, Jiajun; Sun, Yong

2016-01-01

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. PMID:27812463

A Quick Method for Determining the Density of Single Crystals.

ERIC Educational Resources Information Center

Roman, Pascual; Gutierrez-Zorrilla, Juan M.

1985-01-01

Shows how the Archimedes method is used to determine the density of a single crystal of ammonium oxalate monohydrate. Also shows how to calculate the density of other chemicals when they are available as single crystals. Experimental procedures and materials needed are included. (JN)

Feasibility of one-shot-per-crystal structure determination using Laue diffraction

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

Cornaby, Sterling; CHESS; Szebenyi, Doletha M. E.

Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Lauemore » technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used.« less

Crystal growth and characterization of bulk Sb2Te3 topological insulator

NASA Astrophysics Data System (ADS)

Sultana, Rabia; Gurjar, Ganesh; Patnaik, S.; Awana, V. P. S.

2018-04-01

The Sb2Te3 crystals are grown using the conventional self flux method via solid state reaction route, by melting constituent elements (Sb and Te) at high temperature (850 °C), followed by slow cooling (2 °C/h). As grown Sb2Te3 crystals are analysed for various physical properties by x-ray diffraction (XRD), Raman Spectroscopy, Scanning Electron Microscopy (SEM) coupled with Energy Dispersive x-ray Spectroscopy (EDAX) and electrical measurements under magnetic field (6 Tesla) down to low temperature (2.5 K). The XRD pattern revealed the growth of synthesized Sb2Te3 sample along (00l) plane, whereas the SEM along with EDAX measurements displayed the layered structure with near stoichiometric composition, without foreign contamination. The Raman scattering studies displayed known ({{{{A}}}1{{g}}}1, {{{{E}}}{{g}}}2 and {{{{A}}}1{{g}}}2) vibrational modes for the studied Sb2Te3. The temperature dependent electrical resistivity measurements illustrated the metallic nature of the as grown Sb2Te3 single crystal. Further, the magneto—transport studies represented linear positive magneto-resistance (MR) reaching up to 80% at 2.5 K under an applied field of 6 Tesla. The weak anti localization (WAL) related low field (±2 Tesla) magneto-conductance at low temperatures (2.5 K and 20 K) has been analysed and discussed using the Hikami—Larkin—Nagaoka (HLN) model. Summarily, the short letter reports an easy and versatile method for crystal growth of bulk Sb2Te3 topological insulator (TI) and its brief physical property characterization.

Hydrolytic weakening in olivine single crystals

NASA Astrophysics Data System (ADS)

Tielke, Jacob A.; Zimmerman, Mark E.; Kohlstedt, David L.

2017-05-01

Deformation experiments on single crystals of San Carlos olivine under hydrous conditions were performed to investigate the microphysical processes responsible for hydrolytic weakening during dislocation creep. Hydrogen was supplied to the crystals using either talc or brucite sealed in nickel capsules with the crystal. Deformation experiments were carried out using a gas medium apparatus at temperatures of 1050° to 1250°C, a confining pressure of 300 MPa, differential stresses of 45 to 294 MPa, and resultant strain rates of 1.5 × 10-6 to 4.4 × 10-4 s-1. For talc-buffered (i.e., water and orthopyroxene-buffered) samples at high temperatures, the dependence of strain rate on stress follows a power law relationship with a stress exponent (n) of ˜2.5 and an activation energy of ˜490 kJ/mol. Brucite-buffered samples deformed faster than talc-buffered samples but contained similar hydrogen concentrations, demonstrating that strain rate is influenced by orthopyroxene activity under hydrous conditions. The values of n and dependence of strain rate on orthopyroxene activity are consistent with hydrolytic weakening occurring in the climb-controlled dislocation creep regime that is associated with deformation controlled by lattice diffusion under hydrous conditions and by pipe diffusion under anhydrous conditions. Analyses of postdeformation electron-backscatter diffraction data demonstrate that dislocations with [100] Burgers vectors are dominant in the climb-controlled regime and dislocations with [001] are dominant in the glide-controlled regime. Comparison of the experimentally determined constitutive equations demonstrates that under hydrous conditions crystals deform 1 to 2 orders of magnitude faster than under anhydrous conditions.

Extreme magnetoresistance and SdH oscillation in compensated semimetals of NbSb2 single crystals

NASA Astrophysics Data System (ADS)

Guo, Lei; Liu, Yu-Kuai; Gao, Guan-Yin; Huang, Ye-Yu; Gao, Heng; Chen, Lei; Zhao, Weiyao; Ren, Wei; Li, Shi-Yan; Li, Xiao-Guang; Dong, Shuai; Zheng, Ren-Kui

2018-04-01

Topological semimetals represent one of the most interesting classes of materials that continue to attract worldwide interest. Here, we report magnetotransport properties of MPn2-type (M = Nb, Ta; Pn = P, As, Sb) NbSb2 single-crystal semimetals with a centrosymmetric C12/m1 space group, paramagnetic ground state, and non-saturation parabolic-like magnetoresistance. The NbSb2 crystals show metallic conductivity down to 2 K and undergo a metal-to-insulator-like transition under a magnetic field B (B ≥ 4 T) and exhibit a resistivity plateau in the low-temperature region (T ≤ 10 K), where the value of resistivity strongly depends on the magnitude and direction of the magnetic field. Upon sweeping the magnetic field from 0 to 14.5 T in the transverse configuration at T = 1.5 K, the NbSb2 crystal shows a large positive magnetoresistance (4.2 × 103% at B = 14.5 T) with Shubnikov-de Haas (SdH) oscillation. Hall measurements reveal that both the carrier compensation between electrons and holes and the high mobility and large mean free path of carriers contribute to the large magnetoresistance. Fast Fourier transform analyses of angle-resolved SdH oscillation indicate that the Fermi surface of the NbSb2 crystal is quasi-two-dimensional with three-dimensional components. These findings, together with the theoretically calculated electronic band structure obtained within the framework of density functional theory, suggest that NbSb2 is a good candidate compensated semimetal for further theoretical and experimental investigation of this family of materials.

Magnetic and Structural Characterization of Fe-Ga Using Kerr Microscopy and Neutron Scattering

DTIC Science & Technology

2010-01-01

117 4.6 Schematic of triple axes single crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right...Therefore, USANS data is one-dimensional. 4.3.3 Single Crystal Neutron Diffraction The single crystal neutron diffractometer, TriCS at Paul Scherrer...crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right) [106] 4.4 Unpolarized SANS In this section, SANS

High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization

NASA Astrophysics Data System (ADS)

Saidaminov, Makhsud I.; Abdelhady, Ahmed L.; Murali, Banavoth; Alarousu, Erkki; Burlakov, Victor M.; Peng, Wei; Dursun, Ibrahim; Wang, Lingfei; He, Yao; Maculan, Giacomo; Goriely, Alain; Wu, Tom; Mohammed, Omar F.; Bakr, Osman M.

2015-07-01

Single crystals of methylammonium lead trihalide perovskites (MAPbX3; MA=CH3NH3+, X=Br- or I-) have shown remarkably low trap density and charge transport properties; however, growth of such high-quality semiconductors is a time-consuming process. Here we present a rapid crystal growth process to obtain MAPbX3 single crystals, an order of magnitude faster than previous reports. The process is based on our observation of the substantial decrease of MAPbX3 solubility, in certain solvents, at elevated temperatures. The crystals can be both size- and shape-controlled by manipulating the different crystallization parameters. Despite the rapidity of the method, the grown crystals exhibit transport properties and trap densities comparable to the highest quality MAPbX3 reported to date. The phenomenon of inverse or retrograde solubility and its correlated inverse temperature crystallization strategy present a major step forward for advancing the field on perovskite crystallization.

Growth of PBI 2 single crystals from stoichiometric and Pb excess melts

NASA Astrophysics Data System (ADS)

Hayashi, T.; Kinpara, M.; Wang, J. F.; Mimura, K.; Isshiki, M.

2008-01-01

We have successfully grown high-purity and -quality PbI 2 single crystals by the vertical Bridgman method. The rocking curves of four-crystal X-ray diffraction (XRD) show 120 arcsec in full-width at half-maximum (FWHM). The photoluminescence (PL) spectra at 7.8 K show the resolved intensive exciton emission line and the weak DAP emission band. The deep-level emissions are not observed. The measurement of the electrical and radiographic properties show that Leadiodide (PbI 2) single crystal has a resistivity of 5×10 10 Ω cm and imager lag is 8 s, respectively. In order to improve the controllability of crystal growth, PbI 2 single crystals were also grown from a lead (Pb) excess PbI 2 source. The experimental results show very good reproducibility. In addition, the growth models of crystal are proposed, and the growth mechanism is discussed.

Solid state parameters, structure elucidation, High Resolution X-Ray Diffraction (HRXRD), phase matching, thermal and impedance analysis on L-Proline trichloroacetate (L-PTCA) NLO single crystals.

PubMed

Kalaiselvi, P; Raj, S Alfred Cecil; Jagannathan, K; Vijayan, N; Bhagavannarayana, G; Kalainathan, S

2014-11-11

Nonlinear optical single crystal of L-Proline trichloroacetate (L-PTCA) was successfully grown by Slow Evaporation Solution Technique (SEST). The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm the structure. From the single crystal XRD data, solid state parameters were determined for the grown crystal. The crystalline perfection has been evaluated using high resolution X-ray diffractometer. The frequencies of various functional groups were identified from FTIR spectral analysis. The percentage of transmittance was obtained from UV Visible spectral analysis. TGA-DSC measurements indicate the thermal stability of the crystal. The dielectric constant, dielectric loss and ac conductivity were measured by the impedance analyzer. The DC conductivity was calculated by the cole-cole plot method. Copyright © 2014 Elsevier B.V. All rights reserved.

Hematite-Ilmenite with Magnetite from the Ecstall Pluton, British Columbia: Single Crystal Magnetic Experiments

NASA Astrophysics Data System (ADS)

Scott, G. R.; Brownlee, S. J.; Feinberg, J. M.; Renne, P. R.

2008-12-01

Rocks provide a compound paleomagnetic signal from mixtures of various iron minerals with different grain sizes and magnetic stabilities. To unravel this complex signal, specific mineral phases with stable remanence can be individually examined as single crystals. In the case of the Ecstall Pluton (~91 Ma), intra-pluton discordance of paleomagnetic directions may be the result of post-crystallization deformation, or mineralogical changes caused by re-heating from the adjacent Quottoon Pluton (~52 Ma). In order to distinguish between these two hypotheses we conducted rock magnetic experiments on single crystals of finely-exsolved hematite-ilmenite along a transect approaching the Quottoon Pluton. Reflected light, and SEM observations show grains of hematite and ilmenite as the dominant Fe-oxide throughout the Ecstall. Nearest the Quottoon Pluton, the hematite-ilmenite grains exhibit the classic rutile blitz texture. The lamellar microstructure observed in the hematite-ilmenite grains, as well as the rutile blitz texture are linked to the thermal history of the Ecstall Pluton, and have important effects on the magnetic properties of these grains (i.e. lamellar magnetism). Our results include the magnetic unmixing of isothermal remanence magnetization (IRM) acquisition, First Order Reversal Curve (FORC) diagrams, temperature vs. remanence experiments (MPMS), and TEM studies. These data provide a spatially resolved record of rock magnetic variations across the Ecstall Pluton, showing evidence of thermally activated reduction of hematite to magnetite in samples within 13 km of the Quottoon Pluton. TEM analysis shows the magnetite is present as 20-50 nm-sized particles within hematite. This mineralogic change may be responsible for the variations in paleomagnetic directions across the Ecstall Pluton, and clear evidence for this reaction cannot be found by traditional rock characterization techniques, illustrating the need to couple detailed rock magnetic, paleomagnetic, and mineralogic analyses.

Selective Metal Cation Capture by Soft Anionic Metal-Organic Frameworks via Drastic Single-Crystal-to-Single-Crystal Transformations

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

Tian, Jian; Saraf, Laxmikant V.; Schwenzer, Birgit

2012-05-25

Flexible anionic metal-organic frameworks transform to neutral heterobimetallic systems via single-crystal-to-single-crystal processes invoked by cation insertion. These transformations are directed by cooperative bond breakage and formation, resulting in expansion or contraction of the 3D framework by up to 33% due to the flexible nature of the organic linker. These MOFs displays highly selective uptake of divalent transition metal cations (Co2+ and Ni2+ for example) over alkali metal cations (Li+ and Na+).

Erbium Distribution in Single Crystal YAG Fibers Grown by Laser-Heated Pedestal Growth Technique

DTIC Science & Technology

2015-08-28

single crystal YAG fibers grown by laser - heated pedestal growth technique Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host...inserted into a SC YAG tube. This rod-in-tube was used as a preform in our laser -heated pedestal growth (LHPG) apparatus to grow a fiber with a radial...fibers grown by laser -heated pedestal growth technique Report Title Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host material has

Alloy Design Challenge: Development of Low Density Superalloys for Turbine Blade Applications

NASA Technical Reports Server (NTRS)

MacKay, Rebecca A.; Gabb, Timothy P.; Smialek, James L.; Nathal, Michael V.

2009-01-01

New low density single crystal (LDS) alloys have been developed for turbine blade applications, which have the potential for significant improvements in the thrust to weight ratio over current production alloys. An innovative alloying strategy was identified to achieve high temperature creep resistance, alloy density reductions, microstructural stability, and cyclic oxidation resistance. The approach relies on the use of molybdenum (Mo) as a potent solid solution strengthener for the nickel (Ni)-base superalloy; Mo has a density much closer to Ni than other refractory elements, such as rhenium (Re) or tungsten (W). A host of testing and microstructural examinations was conducted on the superalloy single crystals, including creep rupture testing, microstructural stability, cyclic oxidation, and hot corrosion. The paper will provide an overview of the single crystal properties that were generated in this new superalloy design space. The paper will also demonstrate the feasibility of this innovative approach of low density single crystal superalloy design. It will be shown that the best LDS alloy possesses the best attributes of three generations of single crystal alloys: the low density of first-generation single crystal alloys, the excellent oxidation resistance of second-generation single crystal alloys, and a creep strength which exceeds that of second and third generation alloys.

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.

Molecular-dynamic simulations of the thermophysical properties of hexanitrohexaazaisowurtzitane single crystal at high pressures and temperatures

NASA Astrophysics Data System (ADS)

Kozlova, S. A.; Gubin, S. A.; Maklashova, I. V.; Selezenev, A. A.

2017-11-01

Molecular dynamic simulations of isothermal compression parameters are performed for a hexanitrohexaazaisowurtzitane single crystal (C6H6O12N12) using a modified ReaxFF-log reactive force field. It is shown that the pressure-compression ratio curve for a single C6H6O12N12 crystal at constant temperature T = 300 K in pressure range P = 0.05-40 GPa is in satisfactory agreement with experimental compression isotherms obtained for a single C6H6O12N12 crystal. Hugoniot molecular-dynamic simulations of the shock-wave hydrostatic compression of a single C6H6O12N12 crystal are performed. Along with Hugoniot temperature-pressure curves, calculated shock-wave pressure-compression ratios for a single C6H6O12N12 crystal are obtained for a wide pressure range of P = 1-40 GPa. It is established that the percussive adiabat obtained for a single C6H6O12N12 crystal is in a good agreement with the experimental data. All calculations are performed using a LAMMPS molecular dynamics simulation software package that provides a ReaxFF-lg reactive force field to support the approach.

Solvothermal synthesis and structure of 3D frameworks of Nd(III) and Y(III) with thiophene-2,5-dicarboxylate and N,N‧-diethylformamide

NASA Astrophysics Data System (ADS)

Sharma, Swati; Yawer, Mohd; Kariem, Mukaddus; Sheikh, Haq Nawaz

2016-08-01

Two new 3D MOFs [Nd2(TDA)3(DEF)2(H2O)]n (1) and [Y4(TDA)6(DEF)4]n (2) [Thiophene-2,5-dicarboxylic acid (H2TDA) and N,N‧-diethylformamide (DEF)] were synthesized by solvothermal method. They were characterized by elemental analyses, infrared spectroscopy and single crystal X-ray diffraction studies. The two MOFs (1) and (2) belong to the monoclinic system with space group P21/n and C 2 respectively. Structural characterizations by single-crystal X-ray crystallography reveal that 1 and 2 adopt three-dimensional frameworks constructed by cross-linking of rod shaped infinite chain secondary building unit (SBU) by thiophene-2,5-dicarboxylates as linker. These frameworks feature rhomboidal channels, inside which coordinated DEF/H2O solvent molecules are located. DEF plays pivotal role in reaction and design of MOFs. Thermogravimetric analysis shows that both MOFs are thermally robust.

The second peak effect and vortex pinning mechanisms in Ba(Fe,Ni)2As2 superconductors

NASA Astrophysics Data System (ADS)

Ghorbani, S. R.; Arabi, H.; Wang, X. L.

2017-09-01

Vortex pinning mechanisms have been studied systematically in BaFe1.9Ni0.1As2 single crystal as a function of temperature and magnetic field. The obtained shielding current density, Js, showed a second peak in the intermediate magnetic field range at high temperatures. The temperature dependence of the shielding current density, Js(T), was analysed within the collective pinning model at different magnetic fields. It was found that the second peak reflects the coexistence of both δl pinning, reflecting spatial variation in the mean free path (l), and δTc pinning, reflecting spatial variation in the superconducting critical temperature (Tc) at low temperature and low magnetic fields in BaFe1.9Ni0.1As2 single crystal. The results clearly show that pinning mechanism effects are strongly temperature and magnetic field dependent, and the second peak effect is more powerful at higher temperatures and magnetic fields. It was also found that the magnetic field mainly controls the pinning mechanism effect.

Dopant activation in Sn-doped Ga2O3 investigated by X-ray absorption spectroscopy

NASA Astrophysics Data System (ADS)

Siah, S. C.; Brandt, R. E.; Lim, K.; Schelhas, L. T.; Jaramillo, R.; Heinemann, M. D.; Chua, D.; Wright, J.; Perkins, J. D.; Segre, C. U.; Gordon, R. G.; Toney, M. F.; Buonassisi, T.

2015-12-01

Doping activity in both beta-phase (β-) and amorphous (a-) Sn-doped gallium oxide (Ga2O3:Sn) is investigated by X-ray absorption spectroscopy (XAS). A single crystal of β-Ga2O3:Sn grown using edge-defined film-fed growth at 1725 °C is compared with amorphous Ga2O3:Sn films deposited at low temperature (<300 °C). Our XAS analyses indicate that activated Sn dopant atoms in conductive single crystal β-Ga2O3:Sn are present as Sn4+, preferentially substituting for Ga at the octahedral site, as predicted by theoretical calculations. In contrast, inactive Sn atoms in resistive a-Ga2O3:Sn are present in either +2 or +4 charge states depending on growth conditions. These observations suggest the importance of growing Ga2O3:Sn at high temperature to obtain a crystalline phase and controlling the oxidation state of Sn during growth to achieve dopant activation.

Experiment and density functional theory analyses of GdTaO4 single crystal

NASA Astrophysics Data System (ADS)

Ding, Shoujun; Kinross, Ashlie; Wang, Xiaofei; Yang, Huajun; Zhang, Qingli; Liu, Wenpeng; Sun, Dunlu

2018-05-01

GdTaO4 is a type of excellent materials that can be used as scintillation, laser matrix as well as self-activated phosphor has generated significant interest. Whereas its band structure, electronic structure and optical properties are still need elucidation. To solve this intriguing problem, high-quality GdTaO4 single crystal (M-type) was grown successfully using Czochralski method. Its structure as well as optical properties was determined in experiment. Moreover, a systematic theoretical calculation based on the density function theory methods were performed on M-type and M‧-type GdTaO4 and their band structure, density of state as well as optical properties were obtained. Combine with the performed experiment results, the calculated results were proved with high reliability. Hence, the calculated results obtained in this work could provide a deep understanding of GdTaO4 material, which also useful for the further investigation on GdTaO4 material.

Crystal growth, piezoelectric, non-linear optical and mechanical properties of lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

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

2017-05-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution growth technique at 35 °C. Single crystal X-ray diffraction study showed that the grown crystal belongs to the triclinic system with space group P1. The mechanical strength decreases with increasing load. The piezoelectric coefficient is found to be 1.41 pC/N. The nonlinear optical property was measured using Kurtz Perry powder technique and SHG efficiency was almost equal to that of KDP.

ACTIVE MEDIA: BaY2F8 single crystals doped with rare-earth ions as promising up-conversion media for UV and VUV lasers

NASA Astrophysics Data System (ADS)

Pushkar', A. A.; Uvarova, T. V.; Molchanov, V. N.

2008-04-01

BaY2F8 crystals are studied as promising active media for UV and VUV lasers. The up-conversion pumping of rare-earth activators is proposed to solve problems related to the solarisation of the medium and the selection of pump sources. The technology of growing oriented BaY2F8 single crystals is developed and the influence of the crystal orientation on the growth rate and quality of single crystals is determined.

Diffusion barrier properties of single- and multilayered quasi-amorphous tantalum nitride thin films against copper penetration

NASA Astrophysics Data System (ADS)

Chen, G. S.; Chen, S. T.

2000-06-01

Tantalum-related thin films containing different amounts of nitrogen are sputter deposited at different argon-to-nitrogen flow rate ratios on (100) silicon substrates. Using x-ray diffractometry, transmission electron microscopy, composition and resistivity analyses, and bending-beam stress measurement technique, this work examines the impact of varying the nitrogen flow rate, particularly on the crystal structure, composition, resistivity, and residual intrinsic stress of the deposited Ta2N thin films. With an adequate amount of controlled, reactive nitrogen in the sputtering gas, thin films of the tantalum nitride of nominal formula Ta2N are predominantly amorphous and can exist over a range of nitrogen concentrations slightly deviated from stoichiometry. The single-layered quasi-amorphous Ta2N (a-Ta2N) thin films yield intrinsic compressive stresses in the range 3-5 GPa. In addition, the use of the 40-nm-thick a-Ta2N thin films with different nitrogen atomic concentrations (33% and 36%) and layering designs as diffusion barriers between silicon and copper are also evaluated. When subjected to high-temperature annealing, the single-layered a-Ta2N barrier layers degrade primarily by an amorphous-to-crystalline transition of the barrier layers. Crystallization of the single-layered stoichiometric a-Ta2N (Ta67N33) diffusion barriers occurs at temperatures as low as 450 °C. Doing so allows copper to preferentially penetrate through the grain boundaries or thermal-induced microcracks of the crystallized barriers and react with silicon, sequentially forming {111}-facetted pyramidal Cu3Si precipitates and TaSi2 Overdoping nitrogen into the amorphous matrix can dramatically increase the crystallization temperature to 600 °C. This temperature increase slows down the inward diffusion of copper and delays the formation of both silicides. The nitrogen overdoped Ta2N (Ta64N36) diffusion barriers can thus be significantly enhanced so as to yield a failure temperature 100 °C greater than that of the Ta67N33 diffusion barriers. Moreover, multilayered films, formed by alternately stacking the Ta67N33 and Ta64N36 layers with an optimized bilayer thickness (λ) of 10 nm, can dramatically reduce the intrinsic compressive stress to only 0.7 GPa and undergo high-temperature annealing without crystallization. Therefore, the Ta67N33/Ta64N36 multilayered films exhibit a much better barrier performance than the highly crystallization-resistant Ta64N36 single-layered films.

The Crystal Hotel: A Microfluidic Approach to Biomimetic Crystallization.

PubMed

Gong, Xiuqing; Wang, Yun-Wei; Ihli, Johannes; Kim, Yi-Yeoun; Li, Shunbo; Walshaw, Richard; Chen, Li; Meldrum, Fiona C

2015-12-02

A "crystal hotel" microfluidic device that allows crystal growth in confined volumes to be studied in situ is used to produce large calcite single crystals with predefined crystallographic orientation, microstructure, and shape by control of the detailed physical environment, flow, and surface chemistry. This general approach can be extended to form technologically important, nanopatterned single crystals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The tensile effect on crack formation in single crystal silicon irradiated by intense pulsed ion beam

NASA Astrophysics Data System (ADS)

Liang, Guoying; Shen, Jie; Zhang, Jie; Zhong, Haowen; Cui, Xiaojun; Yan, Sha; Zhang, Xiaofu; Yu, Xiao; Le, Xiaoyun

2017-10-01

Improving antifatigue performance of silicon substrate is very important for the development of semiconductor industry. The cracking behavior of silicon under intense pulsed ion beam irradiation was studied by numerical simulation in order to understand the mechanism of induced surface peeling observed by experimental means. Using molecular dynamics simulation based on Stillinger Weber potential, tensile effect on crack growth and propagation in single crystal silicon was investigated. Simulation results reveal that stress-strain curves of single crystal silicon at a constant strain rate can be divided into three stages, which are not similar to metal stress-strain curves; different tensile load velocities induce difference of single silicon crack formation speed; the layered stress results in crack formation in single crystal silicon. It is concluded that the crack growth and propagation is more sensitive to strain rate, tensile load velocity, stress distribution in single crystal silicon.

Crystal growth of triphenylphosphine oxide 4-nitrophenol (TP4N) for nonlinear optical (NLO) applications

NASA Astrophysics Data System (ADS)

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

2018-04-01

The optically good quality organic single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) were successfully grown by slow evaporation solution technique (SEST) using methanol as solvent. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. The optical transmittance, cut-off wavelength and band gap of the TP4N crystal were obtained by UV-Vis NIR spectrum analysis. The photoluminescence studies were carried out to find out the luminesce properties of TP4N single crystal. The photoconductivity studies reveal that the TP4N crystal has negative photoconductive nature. The third order nonlinear susceptibility (χ(3)) of TP4N crystal was evaluated using the Z-scan technique at 640 nm.

Plastic deformation in nanoscale gold single crystals and open-celled nanoporous gold

NASA Astrophysics Data System (ADS)

Lee, Dongyun; Wei, Xiaoding; Zhao, Manhong; Chen, Xi; Jun, Seong C.; Hone, James; Kysar, Jeffrey W.

2007-01-01

The results of two sets of experiments to measure the elastic-plastic behaviour of gold at the nanometre length scale are reported. One set of experiments was on free-standing nanoscale single crystals of gold, and the other was on free-standing nanoscale specimens of open-celled nanoporous gold. Both types of specimens were fabricated from commercially available leaf which was either pure Au or a Au/Ag alloy following by dealloying of the Ag. Mechanical testing specimens of a 'dog-bone' shape were fabricated from the leaf using standard lithographic procedures after the leaf had been glued onto a silicon wafer. The thickness of the gauge portion of the specimens was about 100 nm, the width between 250 nm and 300 nm and the length 7 µm. The specimens were mechanically loaded with a nanoindenter (MTS) at the approximate midpoint of the gauge length. The resulting force-displacement curve of the single crystal gold was serrated and it was evident that slip localization occurred on individual slip systems; however, the early stages of the plastic deformation occurred in a non-localized manner. The results of detailed finite element analyses of the specimen suggest that the critical resolved shear stress of the gold single crystal was as high as 135 MPa which would lead to a maximum uniaxial stress of about 500 MPa after several per cent strain. The behaviour of the nanoporous gold was substantially different. It exhibited an apparent elastic behaviour until the point where it failed in an apparently brittle manner, although it is assumed that plastic deformation occurred in the ligaments prior to failure. The average elastic stiffness of three specimens was measured to be Enp = 8.8 GPa and the stress at ultimate failure averaged 190 MPa for the three specimens tested. Scaling arguments suggest that the stress in the individual ligaments could approach the theoretical shear strength. Presented at the IUTAM Symposium on Plasticity at the Micron Scale, Technical University of Denmark, Copenhagen, Denmark.

Fabrication of patterned single-crystal SrTiO3 thin films by ion slicing and anodic bonding

NASA Astrophysics Data System (ADS)

Lee, Yoo Seung; Djukic, Djordje; Roth, Ryan M.; Laibowitz, Robert; Izuhara, Tomoyuki; Osgood, Richard M.; Bakhru, Sasha; Bakhru, Hassaram; Si, Weidong; Welch, David

2006-09-01

A new technique for directly fabricating patterned thin films (<1μm thick) of fully single-crystal strontium titanate uses deep H+ implantation into the oxide sample, followed by anodic bonding of the sample to a Pyrex or Pyrex-on-Si substrate. The dielectric properties and crystal structure of such thin films are characterized and are found to be essentially those of the bulk single crystal.

Formation of natural gypsum megacrystals in Naica, Mexico

NASA Astrophysics Data System (ADS)

García-Ruiz, Juan Manuel; Villasuso, Roberto; Ayora, Carlos; Canals, Angels; Otálora, Fermín

2007-04-01

Exploration in the Naica mine (Chihuahua, Mexico) recently unveiled several caves containing giant, faceted, and transparent single crystals of gypsum (CaSO4•2H2O) as long as 11 m. These large crystals form at very low supersaturation. The problem is to explain how proper geochemical conditions can be sustained for a long time without large fluctuations that would trigger substantial nucleation. Fluid inclusion analyses show that the crystals grew from low-salinity solutions at a temperature of ˜54 °C, slightly below the one at which the solubility of anhydrite equals that of gypsum. Sulfur and oxygen isotopic compositions of gypsum crystals are compatible with growth from solutions resulting from dissolution of anhydrite previously precipitated during late hydrothermal mineralization, suggesting that these megacrystals formed by a self-feeding mechanism driven by a solution-mediated, anhydrite-gypsum phase transition. Nucleation kinetics calculations based on laboratory data show that this mechanism can account for the formation of these giant crystals, yet only when operating within the very narrow range of temperature identified by our fluid inclusion study. These singular conditions create a mineral wonderland, a site of scientific interest, and an extraordinary phenomenon worthy of preservation.

Growth and structural characterization of single crystals of the magnetic superconductor Ru1-xSr2-yGd1+yCu2+xO8-δ (RuGd-1212) obtained by the partial melting technique

NASA Astrophysics Data System (ADS)

Yamaki, K.; Bamba, Y.; Mochiku, T.; Funahashi, S.; Matsushita, Y.; Irie, A.

2018-05-01

In this study, cubic single crystals of the magnetic superconductor Ru1-xSr2-yGd1+yCu2+xO8-δ (RuGd-1212) with typical dimensions of 100-150 μm in length were grown by the partial melting technique. Multiple 00l reflections were first observed by XRD measurements of the bulk RuGd-1212 single crystals. The resistivity of the obtained crystals was roughly estimated to be ∼24-80 mΩ cm and no superconducting transition was observed down to 4.2 K. From the XRD measurements and refinement of the crystal structure, it was apparent that the Ru and Sr sites of the single-crystal RuGd-1212 were partially substituted by Cu and Gd, respectively. Oxygen defects were found to be minor (δ ≈ 0.1). The lattice parameters a and c of the single crystals were found to be larger and smaller, respectively, than those of a polycrystalline sample.

Ultratough single crystal boron-doped diamond

DOEpatents

Hemley, Russell J [Carnegie Inst. for Science, Washington, DC ; Mao, Ho-Kwang [Carnegie Inst. for Science, Washington, DC ; Yan, Chih-Shiue [Carnegie Inst. for Science, Washington, DC ; Liang, Qi [Carnegie Inst. for Science, Washington, DC

2015-05-05

The invention relates to a single crystal boron doped CVD diamond that has a toughness of at least about 22 MPa m.sup.1/2. The invention further relates to a method of manufacturing single crystal boron doped CVD diamond. The growth rate of the diamond can be from about 20-100 .mu.m/h.

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

Sornadurai, D.; Ravindran, T. R.; Paul, V. Thomas

Synthesis parameters are optimized in order to grow single crystals of multiferroic BiFeO{sub 3}. 2 to 3 mm size pyramid (tetrahedron) shaped single crystals were successfully obtained by solvothermal method. Scanning electron microscopy with EDAX confirmed the phase formation. Raman scattering spectra of bulk BiFeO3 single crystals have been measured which match well with reported spectra.

Arc-melting preparation of single crystal LaB.sub.6 cathodes

DOEpatents

Gibson, Edwin D.; Verhoeven, John D.

1977-06-21

A method for preparing single crystals of lanthanum hexaboride (LaB.sub.6) by arc melting a rod of compacted LaB.sub.6 powder. The method is especially suitable for preparing single crystal LaB.sub.6 cathodes for use in scanning electron microscopes (SEM) and scanning transmission electron microscopes (STEM).

Deformation Mechanism and Recrystallization Relationships in Galfenol Single Crystals: On the Origin of Goss and Cube Orientations

NASA Astrophysics Data System (ADS)

Na, Suok-Min; Smith, Malcolm; Flatau, Alison B.

2018-06-01

In this work, deformation mechanism related to recrystallization behavior in single-crystal disks of Galfenol (Fe-Ga alloy) was investigated to gain insights into the influence of crystal orientations on structural changes and selective grain growth that take place during secondary recrystallization. We started with the three kinds of single-crystal samples with (011)[100], (001)[100], and (001)[110] orientations, which were rolled and annealed to promote the formation of different grain structures and texture evolutions. The initial Goss-oriented (011)[100] crystal mostly rotated into {111}<112> orientations with twofold symmetry and shear band structures by twinning resulted in the exposure of rolled surface along {001}<110> orientation during rolling. In contrast, the Cube-oriented (001)[100] single crystal had no change in texture during rolling with the thickness reduction up to 50 pct. The {123}<111> slip systems were preferentially activated in these single crystals during deformation as well as {112}<111> slip systems that are known to play a role in primary slip of body-centered cubic (BCC) materials such as α-iron and Fe-Si alloys. After annealing, the deformed Cube-oriented single crystal had a small fraction (<10 pct) of recrystallized Goss-oriented grains. The weak Goss component remained in the shear bands of the 50 pct rolled Goss-oriented single crystal, and it appeared to be associated with coalescence of subgrains inside shear band structures during primary recrystallization. Rolling of the (001)[110] single crystal led to the formation of a tilted (001)[100] component close to the <120> orientation, associated with {123}<111> slip systems as well. This was expected to provide potential sites of nucleation for secondary recrystallization; however, no Goss- and Cube-oriented components actually developed in this sample during secondary recrystallization. Those results illustrated how the recrystallization behavior can be influenced by deformed structure and the slip systems.

Single crystal growth and structural evolution across the 1st order valence transition in (Pr1-yYy)1-xCaxCoO3-δ

NASA Astrophysics Data System (ADS)

Schreiber, N. J.; Zhang, Junjie; Zheng, Hong; Freeland, J. W.; Chen, Yu-Sheng; Mitchell, J. F.; Phelan, D.

2017-10-01

Praseodymium-containing cobalt perovskites, such as (Pr1-yYy)1-xCaxCoO3-δ, have been argued to undergo a first-order charge shift between Pr and hybridized Co-O orbitals that leads to a metal-insulator transition at a temperature, TVT. Magnetization and x-ray absorption spectroscopy measurements on single crystals of (Pr0.85Y0.15)0.7Ca0.3CoO3-δ grown in an IR image furnace under 40-60 bar of oxygen confirm the presence of this valence transition. Single crystal x-ray synchrotron diffraction measurements are consistent with an isomorphic phase transition at TVT. No evidence of charge ordering was revealed by the single crystal diffraction. Dissimilar to analytical transmission electron microscopy measurements performed on a grain from a polycrystalline sample that revealed an oxygen vacancy order-disorder transition at TVT, the present single-crystal measurements did not evidence such a transition, likely reflecting a lower density of oxygen vacancies in the high-pO2 grown single crystals.

Method for implantation of high dopant concentrations in wide band gap materials

DOEpatents

Usov, Igor [Los Alamos, NM; Arendt, Paul N [Los Alamos, NM

2009-09-15

A method that combines alternate low/medium ion dose implantation with rapid thermal annealing at relatively low temperatures. At least one dopant is implanted in one of a single crystal and an epitaxial film of the wide band gap compound by a plurality of implantation cycles. The number of implantation cycles is sufficient to implant a predetermined concentration of the dopant in one of the single crystal and the epitaxial film. Each of the implantation cycles includes the steps of: implanting a portion of the predetermined concentration of the one dopant in one of the single crystal and the epitaxial film; annealing one of the single crystal and the epitaxial film and implanted portion at a predetermined temperature for a predetermined time to repair damage to one of the single crystal and the epitaxial film caused by implantation and activates the implanted dopant; and cooling the annealed single crystal and implanted portion to a temperature of less than about 100.degree. C. This combination produces high concentrations of dopants, while minimizing the defect concentration.

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

Swinging Symmetry, Multiple Structural Phase Transitions, and Versatile Physical Properties in RECuGa3 (RE = La-Nd, Sm-Gd).

PubMed

Subbarao, Udumula; Rayaprol, Sudhindra; Dally, Rebecca; Graf, Michael J; Peter, Sebastian C

2016-01-19

The compounds RECuGa3 (RE = La-Nd, Sm-Gd) were synthesized by various techniques. Preliminary X-ray diffraction (XRD) analyses at room temperature suggested that the compounds crystallize in the tetragonal system with either the centrosymmetric space group I4/mmm (BaAl4 type) or the non-centrosymmetric space group I4mm (BaNiSn3 type). Detailed single-crystal XRD, neutron diffraction, and synchrotron XRD studies of selected compounds confirmed the non-centrosymmetric BaNiSn3 structure type at room temperature with space group I4mm. Temperature-dependent single-crystal XRD, powder XRD, and synchrotron beamline measurements showed a structural transition between centro- and non-centrosymmetry followed by a phase transition to the Rb5Hg19 type (space group I4/m) above 400 K and another transition to the Cu3Au structure type (space group Pm3̅m) above 700 K. Combined single-crystal and synchrotron powder XRD studies of PrCuGa3 at high temperatures revealed structural transitions at higher temperatures, highlighting the closeness of the BaNiSn3 structure to other structure types not known to the RECuGa3 family. The crystal structure of RECuGa3 is composed of eight capped hexagonal prism cages [RE4Cu4Ga12] occupying one rare-earth atom in each ring, which are shared through the edge of Cu and Ga atoms along the ab plane, resulting in a three-dimensional network. Resistivity and magnetization measurements demonstrated that all of these compounds undergo magnetic ordering at temperatures between 1.8 and 80 K, apart from the Pr and La compounds: the former remains paramagnetic down to 0.3 K, while superconductivity was observed in the La compound at T = 1 K. It is not clear whether this is intrinsic or due to filamentary Ga present in the sample. The divalent nature of Eu in EuCuGa3 was confirmed by magnetization measurements and X-ray absorption near edge spectroscopy and is further supported by the crystal structure analysis.

Preparation and characterization of the magnetic superconductor EuSr2RuCu2O8-δ (RuEu-1212) by partial melting

NASA Astrophysics Data System (ADS)

Yamaki, K.; Kitagawa, N.; Funahashi, S.; Bamba, Y.; Irie, A.

2018-07-01

In this study, fine single crystals of the magnetic superconductor EuSr2RuCu2O8-δ (RuEu-1212) were successfully prepared using the partial melting technique. The obtained single crystals had a cubic shape, which coincides with the results of previous studies of RuGd-1212 single crystals. The single crystals had a typical length of 20-30 μm and the diffraction pattern observed from a sample prepared by partial melting was consistent with patterns of previously reported polycrystalline RuEu-1212 samples. A sample subjected to prolonged sintering, which consisted of a large number of combined micro single crystals prepared by partial melting, exhibited a superconducting transition with Tc-onset of 30.9 K and Tc-zero of 10.5 K.

Thermal effects in equilibrium surface segregation in a copper/10-atomic-percent-aluminum alloy using Auger electron spectroscopy

NASA Technical Reports Server (NTRS)

Ferrante, J.

1972-01-01

Equilibrium surface segregation of aluminum in a copper-10-atomic-percent-aluminum single crystal alloy oriented in the /111/ direction was demonstrated by using Auger electron spectroscopy. This crystal was in the solid solution range of composition. Equilibrium surface segregation was verified by observing that the aluminum surface concentration varied reversibly with temperature in the range 550 to 850 K. These results were curve fitted to an expression for equilibrium grain boundary segregation and gave a retrieval energy of 5780 J/mole (1380 cal/mole) and a maximum frozen-in surface coverage three times the bulk layer concentration. Analyses concerning the relative merits of sputtering calibration and the effects of evaporation are also included.

Practical applications of nondestructive materials characterization

NASA Astrophysics Data System (ADS)

Green, Robert E., Jr.

1992-10-01

Nondestructive evaluation (NDE) techniques are reviewed for applications to the industrial production of materials including microstructural, physical, and chemical analyses. NDE techniques addressed include: (1) double-pulse holographic interferometry for sealed-package leak testing; (2) process controls for noncontact metals fabrication; (3) ultrasonic detections of oxygen contamination in titanium welds; and (4) scanning acoustic microscopy for the evaluation of solder bonds. The use of embedded sensors and emerging NDE concepts provides the means for controlling the manufacturing and quality of quartz crystal resonators, nickel single-crystal turbine blades, and integrated circuits. Advances in sensor technology and artificial intelligence algorithms and the use of embedded sensors combine to make NDE technology highly effective in controlling industrial materials manufacturing and the quality of the products.

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.

Corrosion and Passivity Studies with Titanium

DTIC Science & Technology

1955-09-30

the (00.1) Face of a Titanium Single Crystal . - Part 3 Secondary Electron Emission from the Titanium Crystal , and from the Copper-Covered Titanium...ner upon the (00.1) face of a titaniuT single crystal . Low- energy electron diffraction is used to investigate the struc- ture of the deposit. Before...cathode emisaion is strongly dependent on the work function k. 8ince varies with crystal faces and the tip is generally so small that it is a single

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

Kuz'mina, L. G., E-mail: kuzmina@igic.ras.ru; Vedernikov, A. I.; Sazonov, S. K.

The crystal packing of a number of styryl dyes of the pyridine series is analyzed. The structures of three dyes and three [2 + 2] photocycloaddition (PCA) products, 1,2,3,4-tetrasubstituted cyclobutanes, obtained in single crystals are determined by X-ray diffraction. Stacks of planar organic cations are characteristic of styryl dye packings. The proceeding of the PCA reaction as a single crystal-to-single crystal transformation in the syn head-to-head stacks is in principle impossible. The syn head-to-tail stacking packings are favorable for the PCA reactions resulting in the centrosymmetric rctt isomers of cyclobutane. The stacking packings, in which molecules are related by themore » twofold axes (the anti arrangement of molecules), are also favorable for PCA in single crystals. In this case, the products are the rtct isomers of cyclobutane. The presence of the I{sup -} counterions in a packing is a factor impeding the PCA reaction, because the secondary I-H-C bonds increase the rigidity of the crystal lattice. The conditions necessary for proceeding the PCA reactions in styryl dyes as single crystal-to-single crystal processes are as follows: (1) the stacks split into pairs of organic cations (dimers) with the d distances within 4.2 A in a dimer and d exceeding 4.2 A between the dimers; and (2) the dimers are surrounded by flexible shells consisting of anions, solvate molecules, or flexible moieties of the organic cations themselves.« less

Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

NASA Astrophysics Data System (ADS)

Ramos, Christian Paul L.; Conato, Marlon T.

2018-05-01

Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

KAMO: towards automated data processing for microcrystals.

PubMed

Yamashita, Keitaro; Hirata, Kunio; Yamamoto, Masaki

2018-05-01

In protein microcrystallography, radiation damage often hampers complete and high-resolution data collection from a single crystal, even under cryogenic conditions. One promising solution is to collect small wedges of data (5-10°) separately from multiple crystals. The data from these crystals can then be merged into a complete reflection-intensity set. However, data processing of multiple small-wedge data sets is challenging. Here, a new open-source data-processing pipeline, KAMO, which utilizes existing programs, including the XDS and CCP4 packages, has been developed to automate whole data-processing tasks in the case of multiple small-wedge data sets. Firstly, KAMO processes individual data sets and collates those indexed with equivalent unit-cell parameters. The space group is then chosen and any indexing ambiguity is resolved. Finally, clustering is performed, followed by merging with outlier rejections, and a report is subsequently created. Using synthetic and several real-world data sets collected from hundreds of crystals, it was demonstrated that merged structure-factor amplitudes can be obtained in a largely automated manner using KAMO, which greatly facilitated the structure analyses of challenging targets that only produced microcrystals. open access.

N-2-Hydroxy-4-methoxyacetophenone- N'-4-nitrobenzoyl hydrazine: Synthesis and structural characterization

NASA Astrophysics Data System (ADS)

Bessy Raj, B. N.; Kurup, M. R. Prathapachandra

2007-04-01

A new aroyl hydrazone, N-2-hydroxy-4-methoxyacetophenone- N'-4-nitrobenzoyl hydrazine was prepared by the condensation reaction of 2-hydroxy-4-methoxyacetophenone and 4-nitrobenzoyl hydrazine. Characterization of the compound was done by elemental analysis and electronic, infrared and NMR spectral analyses. The complete structural assignment of the compound was done by NMR studies by using COSY homonuclear and HSQC heteronuclear techniques. The crystal and molecular structure was determined by single crystal X-ray diffraction studies: crystallized in the monoclinic system, space group P2 1/ n, Z = 4, a = 7.3343(9) Å, b = 20.3517(9) Å, c = 10.1375(5) Å, α = 90.00°, β = 95.735(7)° and γ = 90.00°. From the crystal structure, it is concluded that the compound exists as the keto isomer in the solid state. There is a completely extended conformation in the central part of the molecule C5 sbnd C8 dbnd N1 sbnd N2 sbnd C10 dbnd O2 with an E configuration at the double bond of the hydrazinic bridge.

Growth and electrical properties of (Mn,F) co-doped 0.92Pb(Zn 1/3Nb 2/3)O 3-0.08PbTiO 3 single crystal

NASA Astrophysics Data System (ADS)

Zhang, Shujun; Lebrun, Laurent; Randall, Clive A.; Shrout, Thomas R.

2004-06-01

The growth and characterization of (Mn,F) doped Pb(Zn 1/3Nb 2/3)O 3-PbTiO 3 (PZNT) single crystals are reported in this paper. The typical single crystal obtained is up to 30 mm size with dark brown color. The crystal lattice parameters of doped PZNT crystal are slightly decreased compared to the pure one. The room temperature dielectric permittivity along <0 0 1> direction is about 6000, which is lower than that of the pure PZNT8 because of the dopants. The Curie temperature of the doped crystal is about 180°C while the ferroelectric phase transition temperature is around 100°C, which are higher than those of the pure PZNT8 single crystal. The remnant polarization and coercive field of <0 0 1> oriented doped crystal measured at 1 Hz and 10 kV/cm field are about 27 μC/cm 2 and 4.2 kV/cm, respectively. The room temperature mechanical quality factor is ˜300. Piezoelectric coefficient of <0 0 1> oriented doped crystal is higher than 3500 pC/N and the longitudinal electromechanical coupling factor is larger than 93%. The piezoelectric properties of doped PZNT single crystal with temperature and orientations are also reported in this paper. The valence state of the manganese dopant was determined by electron spin resonance, indicating no Mn 4+ in the crystals, suggesting the valence of manganese ions in PZNT crystals may be 2+, which acts as a hardener, stabilizes the domain wall and pins the domain wall motion, on the other hand, the dopant will enter Ti 4+ position, shifting the crystal composition to higher PT content.

Light emission from organic single crystals operated by electrolyte doping

NASA Astrophysics Data System (ADS)

Matsuki, Keiichiro; Sakanoue, Tomo; Yomogida, Yohei; Hotta, Shu; Takenobu, Taishi

2018-03-01

Light-emitting devices based on electrolytes, such as light-emitting electrochemical cells (LECs) and electric double-layer transistors (EDLTs), are solution-processable devices with a very simple structure. Therefore, it is necessary to apply this device structure into highly fluorescent organic materials for future printed applications. However, owing to compatibility problems between electrolytes and organic crystals, electrolyte-based single-crystal light-emitting devices have not yet been demonstrated. Here, we report on light-emitting devices based on organic single crystals and electrolytes. As the fluorescent materials, α,ω-bis(biphenylyl)terthiophene (BP3T) and 5,6,11,12-tetraphenylnaphthacene (rubrene) single crystals were selected. Using ionic liquids as electrolytes, we observed clear light emission from BP3T LECs and rubrene EDLTs.

Eutectic Formation During Solidification of Ni-Based Single-Crystal Superalloys with Additional Carbon

NASA Astrophysics Data System (ADS)

Wang, Fu; Ma, Dexin; Bührig-Polaczek, Andreas

2017-11-01

γ/ γ' eutectics' nucleation behavior during the solidification of a single-crystal superalloy with additional carbon was investigated by using directional solidification quenching method. The results show that the nucleation of the γ/ γ' eutectics can directly occur on the existing γ dendrites, directly in the remaining liquid, or on the primary MC-type carbides. The γ/γ' eutectics formed through the latter two mechanisms have different crystal orientations than that of the γ matrix. This suggests that the conventional Ni-based single-crystal superalloy castings with additional carbon only guarantee the monocrystallinity of the γ matrix and some γ/ γ' eutectics and, in addition to the carbides, there are other misoriented polycrystalline microstructures existing in macroscopically considered "single-crystal" superalloy castings.

Self-cavity lasing in optically pumped single crystals of p-sexiphenyl

NASA Astrophysics Data System (ADS)

Yanagi, Hisao; Tamura, Kenji; Sasaki, Fumio

2016-08-01

Organic single-crystal self-cavities are prepared by solution growth of p-sexiphenyl (p-6P). Based on Fabry-Pérot feedback inside a quasi-lozenge-shaped platelet crystal, edge-emitting laser is obtained under optical pumping. The multimode lasing band appears at the 0-1 or 0-2 vibronic progressions depending on the excitation conditions which affect the self-absorption effect. Cavity-size dependence of amplified spontaneous emission (ASE) is investigated with laser-etched single crystals of p-6P. As the cavity length of square-shaped crystal is reduced from 100 to 10 μm, ASE threshold fluence is decreased probably due to size-dependent light confinement in the crystal cavity.

Micro pulling down growth of very thin shape memory alloys single crystals

NASA Astrophysics Data System (ADS)

López-Ferreño, I.; Juan, J. San; Breczewski, T.; López, G. A.; Nó, M. L.

Shape memory alloys (SMAs) have attracted much attention in the last decades due to their thermo-mechanical properties such as superelasticity and shape memory effect. Among the different families of SMAs, Cu-Al-Ni alloys exhibit these properties in a wide range of temperatures including the temperature range of 100-200∘C, where there is a technological demand of these functional materials, and exhibit excellent behavior at small scale making them more competitive for applications in Micro Electro-Mechanical Systems (MEMS). However, polycrystalline alloys of Cu-based SMAs are very brittle so that they show their best thermo-mechanical properties in single-crystal state. Nowadays, conventional Bridgman and Czochralski methods are being applied to elaborate single-crystal rods up to a minimum diameter of 1mm, but no works have been reported for smaller diameters. With the aim of synthesizing very thin single-crystals, the Micro-Pulling Down (μ-PD) technique has been applied, for which the capillarity and surface tension between crucible and the melt play a critical role. The μ-PD method has been successfully applied to elaborate several cylindrical shape thin single-crystals down to 200μm in diameter. Finally, the martensitic transformation, which is responsible for the shape memory properties of these alloys, has been characterized for different single-crystals. The experimental results evidence the good quality of the grown single-crystals.

Magnetic field controlled floating-zone single crystal growth of intermetallic compounds

NASA Astrophysics Data System (ADS)

Hermann, R.; Gerbeth, G.; Priede, J.

2013-03-01

Radio-frequency (RF) floating zone single crystal growth is an important technique for the preparation of single bulk crystals. The advantage of the floating-zone method is the crucible-free growth of single crystals of reactive materials with high melting points. The strong heat diffusion on the surface, as well as the melt convection in the molten zone due to induction heating, often leads to an undesired solid-liquid interface geometry with a concave (towards the solid phase) outer rim. These concave parts aggravate the single crystal growth over the full cross-section. A two-phase stirrer was developed at IFW Dresden in order to avoid the problems connected with these concave parts. It acts as a magnetic field pump and changes the typical double vortex structure to a single roll structure, thus pushing hot melt into the regions where the concave parts may arise. The current in the secondary coil is induced by the primary coil, and the capacitor and the resistance of the secondary circuit are adjusted to get a stable 90 degree phase-shift between the coil currents. Single crystal growth of industrial relevant RuAl and TiAl intermetallic compounds was performed based on the material parameters and using the adjusted two-phase stirrer. Very recently, the magnetic system was applied to the crystal growth of biocompatible TiNb alloys and antiferromagnetic Heusler MnSi compounds.

High Performance Relaxor-Based Ferroelectric Single Crystals for Ultrasonic Transducer Applications

PubMed Central

Chen, Yan; Lam, Kwok-Ho; Zhou, Dan; Yue, Qingwen; Yu, Yanxiong; Wu, Jinchuan; Qiu, Weibao; Sun, Lei; Zhang, Chao; Luo, Haosu; Chan, Helen L. W.; Dai, Jiyan

2014-01-01

Relaxor-based ferroelectric single crystals Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT) have drawn much attention in the ferroelectric field because of their excellent piezoelectric properties and high electromechanical coupling coefficients (d33∼2000 pC/N, kt∼60%) near the morphotropic phase boundary (MPB). Ternary Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 (PIN-PMN-PT) single crystals also possess outstanding performance comparable with PMN-PT single crystals, but have higher phase transition temperatures (rhombohedral to tetragonal Trt, and tetragonal to cubic Tc) and larger coercive field Ec. Therefore, these relaxor-based single crystals have been extensively employed for ultrasonic transducer applications. In this paper, an overview of our work and perspectives on using PMN-PT and PIN-PMN-PT single crystals for ultrasonic transducer applications is presented. Various types of single-element ultrasonic transducers, including endoscopic transducers, intravascular transducers, high-frequency and high-temperature transducers fabricated using the PMN-PT and PIN-PMN-PT crystals and their 2-2 and 1-3 composites are reported. Besides, the fabrication and characterization of the array transducers, such as phased array, cylindrical shaped linear array, high-temperature linear array, radial endoscopic array, and annular array, are also addressed. PMID:25076222

Bio-inspired formation of functional calcite/metal oxide nanoparticle composites.

PubMed

Kim, Yi-Yeoun; Schenk, Anna S; Walsh, Dominic; Kulak, Alexander N; Cespedes, Oscar; Meldrum, Fiona C

2014-01-21

Biominerals are invariably composite materials, where occlusion of organic macromolecules within single crystals can significantly modify their properties. In this article, we take inspiration from this biogenic strategy to generate composite crystals in which magnetite (Fe3O4) and zincite (ZnO) nanoparticles are embedded within a calcite single crystal host, thereby endowing it with new magnetic or optical properties. While growth of crystals in the presence of small molecules, macromolecules and particles can lead to their occlusion within the crystal host, this approach requires particles with specific surface chemistries. Overcoming this limitation, we here precipitate crystals within a nanoparticle-functionalised xyloglucan gel, where gels can also be incorporated within single crystals, according to their rigidity. This method is independent of the nanoparticle surface chemistry and as the gel maintains its overall structure when occluded within the crystal, the nanoparticles are maintained throughout the crystal, preventing, for example, their movement and accumulation at the crystal surface during crystal growth. This methodology is expected to be quite general, and could be used to endow a wide range of crystals with new functionalities.

A study of crystal growth by solution technique. [triglycine sulfate single crystals

NASA Technical Reports Server (NTRS)

Lal, R. B.

1979-01-01

The advantages and mechanisms of crystal growth from solution are discussed as well as the effects of impurity adsorption on the kinetics of crystal growth. Uncertainities regarding crystal growth in a low gravity environment are examined. Single crystals of triglycine sulfate were grown using a low temperature solution technique. Small components were assembled and fabricated for future space flights. A space processing experiment proposal accepted by NASA for the Spacelab-3 mission is included.

Syntheses, crystal structures and magnetic properties of complexes based on [Ni(L-L)3]2+ complex cations with dimethylderivatives of 2,2‧-bipyridine and TCNQ

NASA Astrophysics Data System (ADS)

Černák, Juraj; Hegedüs, Michal; Váhovská, Lucia; Kuchár, Juraj; Šoltésová, Daniela; Čižmár, Erik; Feher, Alexander; Falvello, L. R.

2018-03-01

From the aqueous-methanolic systems Ni(NO3)2 - LiTCNQ - 5,5‧-dmbpy and Ni(NO3)2 - LiTCNQ - 4,4‧-dmbpy three novel complexes [Ni(5,5‧-dmbpy)3](TCNQ)2 (1), [Ni(4,4‧-dmbpy)3](TCNQ)2 (2) and [Ni(4,4‧-dmbpy)3]2(TCNQ-TCNQ)(TCNQ)2•0.60H2O (3), were isolated in single crystal form. The new compounds were identified using chemical analyses and IR spectroscopy. Single crystal studies of all samples corroborated their compositions and have shown that their ionic structures contain the complex cations [Ni(5,5‧-dmbpy)]2+ (1) or [Ni(4,4‧-dmbpy)]2+ (2 and 3). The anionic parts of the respective crystal structures 1-3 are formed by TCNQṡ- anion-radicals and in 3 also by a σ-dimerized dianion (TCNQ-TCNQ)2- with a C-C distance of 1.663(5) Å. The supramolecular structures are governed by weak hydrogen bonding interactions. The variable-temperature (2-300 K) magnetic studies of 1 and 3 confirmed the presence of magnetically active Ni(II) atoms with S = 1 and TCNQṡ- anion-radicals with S = 1/2 while the (TCNQ-TCNQ)2- dianion is magnetically silent. The magnetic behavior was described by a complex magnetic model assuming strong antiferromagnetic interactions between some TCNQṡ- anion-radicals.

Synthesis, growth, structural, optical and thermal properties of an organic single crystal: 4-nitroaniline 4-aminobenzoic acid.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2014-01-24

The organic single crystals of 4-nitroaniline 4-aminobenzoic acid (4NAABA) were grown from ethanol solvent. The lattice parameters of the grown crystal have been confirmed from single crystal XRD analysis. The powder XRD pattern shows the various planes of grown crystal. The FTIR and (1)H NMR spectral analysis confirm the presence of various functional groups and the placement of proton in 4NAABA compound respectively. The UV absorption was carried out which shows the cutoff wavelength around 459 nm. The optical band gap of the crystal has been evaluated from the transmission spectra and absorption coefficient by extrapolation technique. In addition, a fluorescence spectral analysis is carried out for 4NAABA crystals. The thermal properties of crystals were evaluated from thermogravimetrical analysis. It shows that the grown crystal is stable up to 160°C and the crystal has sharp melting point at 151°C. Copyright © 2013 Elsevier B.V. All rights reserved.

Structure cristalline et analyses thermique et de surface Hirshfeld du diperchlorate de 4-aza­niumyl-2,2,6,6-tétraméthylpipéridin-1-ium

PubMed Central

Boumakhla, Abdessalem; Zid, Mohamed Faouzi; Guesmi, Abderrahmen

2017-01-01

The synthesis of 4-aza­niumyl-2,2,6,6-tetra­methyl­piperidin-1-ium diperchlorate, C9H22N2 2+·2ClO4 −, was carried out from an aqueous reaction of perchloric acid with 4-amino-2,2,6,6-tetra­methyl­piperidine. This compound was characterized by TGA–DSC analysis and single-crystal X-ray diffraction. The piperidine ring of the dication adopts a chair conformation and the orientation of the C—NH3 bond is equatorial. One of the two crystallographically independent perchlorate anions exhibits disorder [occupancies 0.625 (7) and 0.375 (7)]. The crystal packing is constituted by a succession of mixed layers parallel to the (-102) plane, made up of C9H22N2 2+ dications and ClO4 − anions. These ions are linked by normal and bifurcated N—H⋯O hydrogen bonds with R 4 4(12) graph-set motifs, generating a two-dimensional network. The inter­molecular inter­actions in the crystal structure were qu­anti­fied and analysed using Hirshfeld surface analysis. PMID:29250357

Three pharmaceuticals cocrystals of adefovir: Syntheses, structures and dissolution study

NASA Astrophysics Data System (ADS)

Zhang, Xiaoming; Sun, Fuxing; Zhang, Tingting; Jia, Jiangtao; Su, Hongmin; Wang, Chenhui; Zhu, Guangshan

2015-11-01

We report here three novel cocrystals, which are composed of adefovir as the API (Active Pharmaceutical Ingredient) with p-aminobenzoic acid (1, 2C8H12N5O4P·C7H6NO2·3H2O), 3,5-dihydroxybenzoic acid (2, C8H12N5O4P·C7H6O4·H2O) and 2,6-pyridinedicarboxlic acid (3, C8H12N5O4P·C7H5NO4) as CCFs (cocrystal formers) respectively by crystal engineering strategy. Their structures were characterized by single crystal X-ray diffraction, powder X-ray diffraction (PXRD) analysis, thermogravimetric analyses (TGA), elemental analysis (EA) and infrared spectral analysis (IR). The analysis of single crystal X-ray diffraction demonstrate that cocrystal 1 and 2 form a strong hydrogen-bonded assembly through the phosphoric acids of API with water in the lattice and carboxylic acids of CCF respectively. Cocrystal 3 is formed in which the phosphoric acid groups of API are also held by the carboxylic acid groups of CCF. The PXRD results indicate their high purity of as-synthesized samples. The TGA, EA, IR and dissolution study of API and the cocrystals were also measured and discussed.

Synthesis, characterization and dissolution of three pharmaceutical cocrystals based on deferiprone

NASA Astrophysics Data System (ADS)

Zhang, Xiaoming; Tian, Yuyang; Jia, Jiangtao; Zhang, Tingting; Zhu, Guangshan

2016-03-01

In this paper we present three new cocrystals based on deferiprone which is the first oral medicine as iron chelator. Solitary deferiprone possesses some known problems due to its good solubility and frequent dosing side effects. For these three novel co crystals, deferiprone is the active pharmaceutical ingredient (API), p-hydroxybenzoic acid (1, C7H9NO2·C7H6O3), 2, 5-dihydroxybenzoic acid (2, C7H9NO2·C7H6O4) and maleic acid (3, C7H9NO2·C4H4O4) are used as cocrystal formers (CCFs), respectively. Their structures were characterized by single crystal X-ray diffraction, powder X-ray diffraction (PXRD) analysis, thermogravimetric analyses (TGA), differential thermal analysis (DTA), elemental analysis (EA) and infrared spectral analysis (IR). Single crystal X-ray diffraction demonstrates that all three cocrystals (1-3) possess strong hydrogen-bondings assembled through hydroxyl of API and carboxylic acids of CCFs. The PXRD results indicate their high purity of as-synthesized samples. TGA, DTA, EA, IR and dissolution study of API and cocrystals were also measured and discussed, respectively. The results suggest that the cocrystals exhibit low dissolution rates comparing with solitary deferiprone, which is very advantageous for the oral medicine with frequent dosing side effects.

Evidence of a 2D Fermi surface due to surface states in a p-type metallic Bi2Te3

NASA Astrophysics Data System (ADS)

Shrestha, K.; Marinova, V.; Lorenz, B.; Chu, C. W.

2018-05-01

We present a systematic quantum oscillations study on a metallic, p-type Bi2Te3 topological single crystal in magnetic fields up to B  =  7 T. The maxima/minima positions of oscillations measured at different tilt angles align to one another when plotted as a function of the normal component of magnetic field, confirming the presence of the 2D Fermi surface. Additionally, the Berry phase, β  =  0.4  ±  0.05 obtained from the Landau level fan plot, is very close to the theoretical value of 0.5 for the Dirac particles, confirming the presence of topological surface states in the Bi2Te3 single crystal. Using the Lifshitz–Kosevich analyses, the Fermi energy is estimated to be meV, which is lower than that of other bismuth-based topological systems. The detection of surface states in the Bi2Te3 crystal can be explained by our previous hypothesis of the lower position of the Fermi surface that cuts the ‘M’-shaped valence band maxima. As a result, the bulk state frequency is shifted to higher magnetic fields, which allows measurement of the surface states signal at low magnetic fields.

Ultra-low thermal conductivity of TlIn5Se8 and structure of the new complex chalcogenide Tl0.98In13.12Se16.7Te2.3

NASA Astrophysics Data System (ADS)

Lefèvre, Robin; Berthebaud, David; Pérez, Olivier; Pelloquin, Denis; Boudin, Sophie; Gascoin, Franck

2017-06-01

TlIn5Se8 has been synthesized by means of solid-state reaction and densified by Spark Plasma Sintering. The compound is a semiconductor with a band gap of 1.62 eV estimated from reflectance measurements. Its thermal conductivity is about 0.45 W m-1. K-1 in the temperature range 300-673 K, an extremely low value attributed to its complex pseudo-1D structure reminiscent of the pseudo-hollandite. While attempting to dope TlIn5Se8 with Te, a new complex chalcogenide was discovered and characterized by the combination of TEM and XRD diffraction. It belongs to the A2In12X19 family, crystallizing in the R 3 ̅:H space group. Single crystal X-ray diffraction study led to a refined composition of Tl0.98In13.12Se16.7Te2.3 with cell parameters: a=13.839(5) Å and c=35.18(3) Å. A static disorder is found on one indium site situated in an octahedral environment. The single crystal XRD study is in agreement with TEM analyses in STEM-HAADF image mode that do not show any extended defects or disorder at atomic scale.

Analysis about diamond tool wear in nano-metric cutting of single crystal silicon using molecular dynamics method

NASA Astrophysics Data System (ADS)

Wang, Zhiguo; Liang, Yingchun; Chen, Mingjun; Tong, Zhen; Chen, Jiaxuan

2010-10-01

Tool wear not only changes its geometry accuracy and integrity, but also decrease machining precision and surface integrity of workpiece that affect using performance and service life of workpiece in ultra-precision machining. Scholars made a lot of experimental researches and stimulant analyses, but there is a great difference on the wear mechanism, especially on the nano-scale wear mechanism. In this paper, the three-dimensional simulation model is built to simulate nano-metric cutting of a single crystal silicon with a non-rigid right-angle diamond tool with 0 rake angle and 0 clearance angle by the molecular dynamics (MD) simulation approach, which is used to investigate the diamond tool wear during the nano-metric cutting process. A Tersoff potential is employed for the interaction between carbon-carbon atoms, silicon-silicon atoms and carbon-silicon atoms. The tool gets the high alternating shear stress, the tool wear firstly presents at the cutting edge where intension is low. At the corner the tool is splitted along the {1 1 1} crystal plane, which forms the tipping. The wear at the flank face is the structure transformation of diamond that the diamond structure transforms into the sheet graphite structure. Owing to the tool wear the cutting force increases.

Simulations of surface stress effects in nanoscale single crystals

NASA Astrophysics Data System (ADS)

Zadin, V.; Veske, M.; Vigonski, S.; Jansson, V.; Muszinsky, J.; Parviainen, S.; Aabloo, A.; Djurabekova, F.

2018-04-01

Onset of vacuum arcing near a metal surface is often associated with nanoscale asperities, which may dynamically appear due to different processes ongoing in the surface and subsurface layers in the presence of high electric fields. Thermally activated processes, as well as plastic deformation caused by tensile stress due to an applied electric field, are usually not accessible by atomistic simulations because of the long time needed for these processes to occur. On the other hand, finite element methods, able to describe the process of plastic deformations in materials at realistic stresses, do not include surface properties. The latter are particularly important for the problems where the surface plays crucial role in the studied process, as for instance, in the case of plastic deformations at a nanovoid. In the current study by means of molecular dynamics (MD) and finite element simulations we analyse the stress distribution in single crystal copper containing a nanovoid buried deep under the surface. We have developed a methodology to incorporate the surface effects into the solid mechanics framework by utilizing elastic properties of crystals, pre-calculated using MD simulations. The method leads to computationally efficient stress calculations and can be easily implemented in commercially available finite element software, making it an attractive analysis tool.

Nanopattern-guided growth of single-crystal silicon on amorphous substrates and high-performance sub-100 nm thin-film transistors for three-dimensional integrated circuits

NASA Astrophysics Data System (ADS)

Gu, Jian

This thesis explores how nanopatterns can be used to control the growth of single-crystal silicon on amorphous substrates at low temperature, with potential applications on flat panel liquid-crystal display and 3-dimensional (3D) integrated circuits. I first present excimer laser annealing of amorphous silicon (a-Si) nanostructures on thermally oxidized silicon wafer for controlled formation of single-crystal silicon islands. Preferential nucleation at pattern center is observed due to substrate enhanced edge heating. Single-grain silicon is obtained in a 50 nm x 100 nm rectangular pattern by super lateral growth (SLG). Narrow lines (such as 20-nm-wide) can serve as artificial heterogeneous nucleation sites during crystallization of large patterns, which could lead to the formation of single-crystal silicon islands in a controlled fashion. In addition to eximer laser annealing, NanoPAtterning and nickel-induced lateral C&barbelow;rystallization (NanoPAC) of a-Si lines is presented. Single-crystal silicon is achieved by NanoPAC. The line width of a-Si affects the grain structure of crystallized silicon lines significantly. Statistics show that single-crystal silicon is formed for all lines with width between 50 nm to 200 nm. Using in situ transmission electron microscopy (TEM), nickel-induced lateral crystallization (Ni-ILC) of a-Si inside a pattern is revealed; lithography-constrained single seeding (LISS) is proposed to explain the single-crystal formation. Intragrain line and two-dimensional defects are also studied. To test the electrical properties of NanoPAC silicon films, sub-100 nm thin-film transistors (TFTs) are fabricated using Patten-controlled crystallization of Ṯhin a-Si channel layer and H&barbelow;igh temperature (850°C) annealing, coined PaTH process. PaTH TFTs show excellent device performance over traditional solid phase crystallized (SPC) TFTs in terms of threshold voltage, threshold voltage roll-off, leakage current, subthreshold swing, on/off current ratio, device-to-device uniformity etc. Two-dimensional device simulations show that PaTH TFTs are comparable to silicon-on-insulator (SOI) devices, making it a promising candidate for the fabrication of future high performance, low-power 3D integrated circuits. Finally, an ultrafast nanolithography technique, laser-assisted direct imprint (LADI) is introduced. LADI shows the ability of patterning nanostructures directly in silicon in nanoseconds with sub-10 nm resolution. The process has potential applications in multiple disciplines, and could be extended to other materials and processes.

Correlating Polymer Crystals via Self-Induced Nucleation

NASA Astrophysics Data System (ADS)

Reiter, Günter

Crystallizable polymers often form multiple stacks of uniquely oriented lamellae, which have good registry despite being separated by amorphous fold surfaces. These correlations require multiple synchronized, yet unidentified, nucleation events. Here, we demonstrate that in thin films of isotactic polystyrene, the probability of generating correlated lamellae is controlled by the branched morphology of a single primary lamella. The nucleation density ns of secondary lamellae is found to be dependent on the width of the branches of the primary lamella. This relation is independent of molecular weight, crystallization temperature, and film thickness. We propose a nucleation mechanism based on the insertion of polymers into a branched primary lamellar crystal. Even in single crystals, characterized by faceted structures with a well-defined envelope reflecting the underlying crystal unit cell, polymers are folded and thus in a meta-stable state. Annealing such meta-stable single crystals allowed to unveil the initial morphological framework of a dendritic single crystal, i.e. the initial stages of growth.

A metamorphic inorganic framework that can be switched between eight single-crystalline states

NASA Astrophysics Data System (ADS)

Zhan, Caihong; Cameron, Jamie M.; Gabb, David; Boyd, Thomas; Winter, Ross S.; Vilà-Nadal, Laia; Mitchell, Scott G.; Glatzel, Stefan; Breternitz, Joachim; Gregory, Duncan H.; Long, De-Liang; MacDonell, Andrew; Cronin, Leroy

2017-02-01

The design of highly flexible framework materials requires organic linkers, whereas inorganic materials are more robust but inflexible. Here, by using linkable inorganic rings made up of tungsten oxide (P8W48O184) building blocks, we synthesized an inorganic single crystal material that can undergo at least eight different crystal-to-crystal transformations, with gigantic crystal volume contraction and expansion changes ranging from -2,170 to +1,720 Å3 with no reduction in crystallinity. Not only does this material undergo the largest single crystal-to-single crystal volume transformation thus far reported (to the best of our knowledge), the system also shows conformational flexibility while maintaining robustness over several cycles in the reversible uptake and release of guest molecules switching the crystal between different metamorphic states. This material combines the robustness of inorganic materials with the flexibility of organic frameworks, thereby challenging the notion that flexible materials with robustness are mutually exclusive.

Experiments on planetary ices at UCL

NASA Astrophysics Data System (ADS)

Grindrod, P. M.; Fortes, A. D.; Wood, I. G.; Dobson, D.; Sammonds, P. R.; Stone-Drake, L.; Vocadlo, L.

2007-08-01

Using a suite of techniques and equipment, we conduct several different types of experiments on planetary ices at UCL. Samples are prepared in the Ice Physics Laboratory, which consists of a 5 chamber complex of inter-connected cold rooms, controllable from +30 to -30 deg C. Within this laboratory we have a functioning triaxial deformation cell operating at low temperature (down to -90 deg C) and high pressures (300 MPa), an Automatic Ice Fabric Analyser (AIFA) and a low-temperature microscope with CCD output. Polycrystalline samples, 40mm diameter by 100mm long, are compressed in the triaxial rig with a confining pressure; single crystal specimens are compressed in a separate uniaxial creep rig which operates at zero confining pressure for surface studies. A cold stage is also available for study of ice microstructural studies on our new Jeol JSM-6480LV SEM, which also allows tensile, compression and/or bending tests, with load ranges from less than 2N to 5000N. Finally, we also use a cold stage on a new PANalytical, X'pert PRO MPD, high resolution powder diffractometer to study the structure and phase behaviour of icy materials. Recent highlights of our work include: (1) derivation of a manufacturing process for methane clathrate at low temperatures, analysed in the X-Ray Diffraction Laboratory, for future rheological experiments, (2) analysed the growth behaviour of MS11, (3) refurbished and commenced calibration tests on the triaxial deformation cell using ice Ih, and (4) performed creep tests on gypsum and epsomite using the single crystal deformation cell. Further experiments will build on these preliminary results.

Oxygen isotope and trace element evidence for three-stage petrogenesis of the youngest episode (260-79 ka) of Yellowstone rhyolitic volcanism

NASA Astrophysics Data System (ADS)

Loewen, Matthew W.; Bindeman, Ilya N.

2015-10-01

We report the first high-precision δ18O analyses of glass, δ18O of minerals, and trace element concentrations in glass and minerals for the 260-79 ka Central Plateau Member (CPM) rhyolites of Yellowstone, a >350 km3 cumulative volume of lavas erupted inside of 630 ka Lava Creek Tuff (LCT) caldera. The glass analyses of these crystal-poor rhyolites provide direct characterization of the melt and its evolution through time. The δ18Oglass values are low and mostly homogeneous (4.5 ± 0.14 ‰) within and in between lavas that erupted in four different temporal episodes during 200 ka of CPM volcanism with a slight shift to lower δ18O in the youngest episode (Pitchstone Plateau). These values are lower than Yellowstone basalts (5.7-6 ‰), LCT (5.5 ‰), pre-, and extracaldera rhyolites (~7-8 ‰), but higher than the earliest 550-450 ka post-LCT rhyolites (1-2 ‰). The glass δ18O value is coupled with new clinopyroxene analyses and previously reported zircon analyses to calculate oxygen isotope equilibration temperatures. Clinopyroxene records >900 °C near-liquidus temperatures, while zircon records temperatures <850 °C similar to zircon saturation temperature estimates. Trace element concentrations in the same glass analyzed for oxygen isotopes show evidence for temporal decreases in Ti, Sr, Ba, and Eu—related to Fe-Ti oxide and sanidine (±quartz) crystallization control, while other trace elements remain similar or are enriched through time. The slight temporal increase in glass Zr concentrations may reflect similar or higher temperature magmas (via zircon saturation) through time, while previosuly reported temperature decreases (e.g., Ti-in-quartz) might reflect changing Ti concentrations with progressive melt evolution. Multiple analyses of glass across single samples and in profiles across lava flow surfaces document trace element heterogeneity with compatible behavior of all analyzed elements except Rb, Nb, and U. These new data provide evidence for a three-stage geochemical evolution of these most recent Yellowstone rhyolites: (1) repeated batch melting events at the base of a homogenized low-δ18O intracaldera fill resulting in liquidus rhyolite melt and a refractory residue that sequesters feldspar-compatible elements over time. This melting may be triggered by conductive "hot plate" heating by basaltic magma intruding beneath the Yellowstone caldera resulting in contact rhyolitic melt that crystallizes early clinopyroxene and/or sanidine at high temperature. (2) Heterogeneity within individual samples and across flows reflects crystallization of these melts during preeruptive storage of magma at at lower, zircon-saturated temperatures. Compatible behavior and variations of most trace elements within individual lava flows are the result of sanidine, quartz, Fe-Ti oxide, zircon, and chevkinite crystallization at this stage. (3) Internal mixing immediately prior to and/or during eruption disrupts, these compositional gradients in each parental magma body that are preserved as melt domains distributed throughout the lava flows. These results based on the most recent and best-preserved volcanic products from the Yellowstone volcanic system provide new insight into the multiple stages required to generate highly fractionated hot spot and rift-related rhyolites. Our proposed model differs from previous interpretations that extreme Sr and Ba depletion result from long-term crystallization of a single magma body—instead we suggest that punctuated batch melting events generated a sanidine-rich refractory residue and a melt source region progressively depleted in Sr and Ba.

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

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.

Dielectric and domain studies on Fe doped KNbO3 single crystal

NASA Astrophysics Data System (ADS)

Shamkuwar, Sanjaykumar H.; Patil, Naresh M.; Korde, Vivek B.; Pradnyakar, Namrata V.

2018-05-01

Synthesis of Fe doped KNbO3 single crystals by flux method is reported here. The effect of Fe-doping on phase transition temperatures of KNbO3 single crystals was investigated using dielectric studies. The phase transition temperatures were found to be 225°C and 425°C which almost same as reported by others. The domain studies were carried out using metallurgical microscope and it shows the presence of 60° and 90° domains in the grown crystals.

Vacuum lamination approach to fabrication of high-performance single-crystal organic field-effect transistors.

PubMed

Yi, H T; Chen, Y; Czelen, K; Podzorov, V

2011-12-22

A novel vacuum lamination approach to fabrication of high-performance single-crystal organic field-effect transistors has been developed. The non-destructive nature of this method allows a direct comparison of field-effect mobilities achieved with various gate dielectrics using the same single-crystal sample. The method also allows gating delicate systems, such as n -type crystals and SAM-coated surfaces, without perturbation. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Defect Initiation/Growth and Energy Dissipation Induced by Deformation and Fracture

DTIC Science & Technology

1993-01-01

deformation in MgO single crystals . 4 III. Molecular CO emission accompanying fracture of polycarbonate: evidence for chain cleavage J. T. Dickinson, L. C... Crystal MgO Although not a polymer, we wish to point out that the fracture-induced phE and EE from the fracture of single crystal MgQ 17 (Fig. 7) is...long times. This is a good qualitative description of the behavior exhibited by EE from in some systems. C. Single Crystal MgO Williams et al. have

Optical characteristics of novel bulk and nanoengineered laser host materials

NASA Astrophysics Data System (ADS)

Prasad, Narasimha S.; Sova, Stacey; Kelly, Lisa; Bevan, Talon; Arnold, Bradley; Cooper, Christopher; Choa, Fow-Sen; Singh, N. B.

2018-02-01

The hexagonal apatite single crystals have been investigated for their applications as laser host materials. Czochralksi and flux growth methods have been utilized to obtain single crystals. For low temperature processing (<100 0C), several techniques for crystal growth have been developed. The hexagonal apatite structure (space group P63/m) is characteristic of several compounds, some of which have extremely interesting and useful properties as laser hosts and bone materials. Calcium lanthanum silicate (Nd-doped) and lanthanum aluminate material systems were studied in detail. Nanoengineered calcium and lanthanum based silicates were synthesized by a solution method and their optical and morphological characteristics were compared with Czochralski grown bulk hydroxyapatite single crystals. Materials were evaluated by absorbance, fluorescence and Raman characteristics. Neodymium, iron and chromium doped crystals grown by a solution method showed weak but similar optical properties to that of Czochralski grown single crystals.

Study on the temperature field of large-sized sapphire single crystal furnace

NASA Astrophysics Data System (ADS)

Zhai, J. P.; Jiang, J. W.; Liu, K. G.; Peng, X. B.; Jian, D. L.; Li, I. L.

2018-01-01

In this paper, the temperature field of large-sized (120kg, 200kg and 300kg grade) sapphire single crystal furnace was simulated. By keeping the crucible diameter ratio and the insulation system unchanged, the power consumption, axial and radial temperature gradient, solid-liquid surface shape, stress distribution and melt flow were studied. The simulation results showed that with the increase of the single crystal furnace size, the power consumption increased, the temperature field insulation effect became worse, the growth stress value increased and the stress concentration phenomenon occurred. To solve these problems, the middle and bottom insulation system should be enhanced during designing the large-sized sapphire single crystal furnace. The appropriate radial and axial temperature gradient was favorable to reduce the crystal stress and prevent the occurrence of cracking. Expanding the interface between the seed and crystal was propitious to avoid the stress accumulation phenomenon.

Large single domain 123 material produced by seeding with single crystal rare earth barium copper oxide single crystals

DOEpatents

Todt, V.; Miller, D.J.; Shi, D.; Sengupta, S.

1998-07-07

A method of fabricating bulk YBa{sub 2}Cu{sub 3}O{sub x} where compressed powder oxides and/or carbonates of Y and Ba and Cu present in mole ratios to form YBa{sub 2}Cu{sub 3}O{sub x} are heated in the presence of a Nd{sub 1+x}Ba{sub 2{minus}x}Cu{sub 3}O{sub y} seed crystal to a temperature sufficient to form a liquid phase in the YBa{sub 2}Cu{sub 3}O{sub x} while maintaining the seed crystal solid. The materials are slowly cooled to provide a YBa{sub 2}Cu{sub 3}O{sub x} material having a predetermined number of domains between 1 and 5. Crack-free single domain materials can be formed using either plate shaped seed crystals or cube shaped seed crystals with a pedestal of preferential orientation material. 7 figs.

Large single domain 123 material produced by seeding with single crystal rare earth barium copper oxide single crystals

DOEpatents

Todt, Volker; Miller, Dean J.; Shi, Donglu; Sengupta, Suvankar

1998-01-01

A method of fabricating bulk YBa.sub.2 Cu.sub.3 O.sub.x where compressed powder oxides and/or carbonates of Y and Ba and Cu present in mole ratios to form YBa.sub.2 Cu.sub.3 O.sub.x are heated in the presence of a Nd.sub.1+x Ba.sub.2-x Cu.sub.3 O.sub.y seed crystal to a temperature sufficient to form a liquid phase in the YBa.sub.2 Cu.sub.3 O.sub.x while maintaining the seed crystal solid. The materials are slowly cooled to provide a YBa.sub.2 Cu.sub.3 O.sub.x material having a predetermined number of domains between 1 and 5. Crack-free single domain materials can be formed using either plate shaped seed crystals or cube shaped seed crystals with a pedestal of preferential orientation material.

Physical and Structural Studies on the Cryo-cooling of Insulin Crystals

NASA Technical Reports Server (NTRS)

Lovelace, J.; Bellamy, H.; Snell, E. H.; Borgstahl, G.

2003-01-01

Reflection profiles were analyzed from microgravity-(mg) and earth-grown insulin crystals to measure mosaicity (h) and to reveal mosaic domain structure and composition. The effects of cryocooling on single and multi-domain crystals were compared. The effects of cryocooling on insulin structure were also re-examined. Microgravity crystals were larger, more homogeneous, and more perfect than earth crystals. Several mg crystals contained primarily a single mosaic domain with havg of 0.005deg. The earth crystals varied in quality and all contained multiple domains with havg of 0.031deg. Cryocooling caused a 43-fold increase in h for mg crystals (havg=0.217deg) and an %fold increase for earth crystals (havg=0.246deg). These results indicate that very well-ordered crystals are not completely protected from the stresses associated with cryocooling, especially when structural perturbations occur. However, there were differences in the reflection profiles. For multi-mosaic domain crystals, each domain individually broadened and separated from the other domains upon cryo-cooling. Cryo-cooling did not cause an increase in the number of domains. A crystal composed of a single domain retained this domain structure and the reflection profiles simply broadened. Therefore, an improved signal-to-noise ratio for each reflection was measured from cryo-cooled single domain crystals relative to cryo-cooled multi-domain crystals. This improved signal, along with the increase in crystal size, facilitated the measurement of the weaker high- resolution reflections. The observed broadening of reflection profiles indicates increased variation in unit cell dimensions which may be linked to cryo-cooling-associated structural changes and disorder.

Repeated growth and bubbling transfer of graphene with millimetre-size single-crystal grains using platinum.

PubMed

Gao, Libo; Ren, Wencai; Xu, Huilong; Jin, Li; Wang, Zhenxing; Ma, Teng; Ma, Lai-Peng; Zhang, Zhiyong; Fu, Qiang; Peng, Lian-Mao; Bao, Xinhe; Cheng, Hui-Ming

2012-02-28

Large single-crystal graphene is highly desired and important for the applications of graphene in electronics, as grain boundaries between graphene grains markedly degrade its quality and properties. Here we report the growth of millimetre-sized hexagonal single-crystal graphene and graphene films joined from such grains on Pt by ambient-pressure chemical vapour deposition. We report a bubbling method to transfer these single graphene grains and graphene films to arbitrary substrate, which is nondestructive not only to graphene, but also to the Pt substrates. The Pt substrates can be repeatedly used for graphene growth. The graphene shows high crystal quality with the reported lowest wrinkle height of 0.8 nm and a carrier mobility of greater than 7,100 cm(2) V(-1) s(-1) under ambient conditions. The repeatable growth of graphene with large single-crystal grains on Pt and its nondestructive transfer may enable various applications.

Repeated growth and bubbling transfer of graphene with millimetre-size single-crystal grains using platinum

PubMed Central

Gao, Libo; Ren, Wencai; Xu, Huilong; Jin, Li; Wang, Zhenxing; Ma, Teng; Ma, Lai-Peng; Zhang, Zhiyong; Fu, Qiang; Peng, Lian-Mao; Bao, Xinhe; Cheng, Hui-Ming

2012-01-01

Large single-crystal graphene is highly desired and important for the applications of graphene in electronics, as grain boundaries between graphene grains markedly degrade its quality and properties. Here we report the growth of millimetre-sized hexagonal single-crystal graphene and graphene films joined from such grains on Pt by ambient-pressure chemical vapour deposition. We report a bubbling method to transfer these single graphene grains and graphene films to arbitrary substrate, which is nondestructive not only to graphene, but also to the Pt substrates. The Pt substrates can be repeatedly used for graphene growth. The graphene shows high crystal quality with the reported lowest wrinkle height of 0.8 nm and a carrier mobility of greater than 7,100 cm2 V−1 s−1 under ambient conditions. The repeatable growth of graphene with large single-crystal grains on Pt and its nondestructive transfer may enable various applications. PMID:22426220

Methodology Developed for Modeling the Fatigue Crack Growth Behavior of Single-Crystal, Nickel-Base Superalloys

NASA Technical Reports Server (NTRS)

1996-01-01

Because of their superior high-temperature properties, gas generator turbine airfoils made of single-crystal, nickel-base superalloys are fast becoming the standard equipment on today's advanced, high-performance aerospace engines. The increased temperature capabilities of these airfoils has allowed for a significant increase in the operating temperatures in turbine sections, resulting in superior propulsion performance and greater efficiencies. However, the previously developed methodologies for life-prediction models are based on experience with polycrystalline alloys and may not be applicable to single-crystal alloys under certain operating conditions. One of the main areas where behavior differences between single-crystal and polycrystalline alloys are readily apparent is subcritical fatigue crack growth (FCG). The NASA Lewis Research Center's work in this area enables accurate prediction of the subcritical fatigue crack growth behavior in single-crystal, nickel-based superalloys at elevated temperatures.

First Point-Spread Function and X-Ray Phase Contrast Imaging Results with an 88-mm Diameter Single Crystal

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

Lumpkin, A. H.; Garson, A. B.; Anastasio, M. A.

In this study, we report initial demonstrations of the use of single crystals in indirect x-ray imaging with a benchtop implementation of propagation-based (PB) x-ray phase contrast imaging. Based on single Gaussian peak fits to the x-ray images, we observed a four times smaller system point-spread function (PSF) with the 50-μm thick single crystal scintillators than with the reference polycrystalline phosphor/scintillator. Fiber-optic plate depth-of-focus and Al reflective-coating aspects are also elucidated. Guided by the results from the 25-mm diameter crystal samples, we report additionally the first results with a unique 88-mm diameter single crystal bonded to a fiber optic platemore » and coupled to the large format CCD. Both PSF and x-ray phase contrast imaging data are quantified and presented.« less

Low-Threshold Lasing from 2D Homologous Organic-Inorganic Hybrid Ruddlesden-Popper Perovskite Single Crystals.

PubMed

Raghavan, Chinnambedu Murugesan; Chen, Tzu-Pei; Li, Shao-Sian; Chen, Wei-Liang; Lo, Chao-Yuan; Liao, Yu-Ming; Haider, Golam; Lin, Cheng-Chieh; Chen, Chia-Chun; Sankar, Raman; Chang, Yu-Ming; Chou, Fang-Cheng; Chen, Chun-Wei

2018-05-09

Organic-inorganic hybrid two-dimensional (2D) perovskites have recently attracted great attention in optical and optoelectronic applications due to their inherent natural quantum-well structure. We report the growth of high-quality millimeter-sized single crystals belonging to homologous two-dimensional (2D) hybrid organic-inorganic Ruddelsden-Popper perovskites (RPPs) of (BA) 2 (MA) n-1 Pb n I 3 n+1 ( n = 1, 2, and 3) by a slow evaporation at a constant-temperature (SECT) solution-growth strategy. The as-grown 2D hybrid perovskite single crystals exhibit excellent crystallinity, phase purity, and spectral uniformity. Low-threshold lasing behaviors with different emission wavelengths at room temperature have been observed from the homologous 2D hybrid RPP single crystals. Our result demonstrates that solution-growth homologous organic-inorganic hybrid 2D perovskite single crystals open up a new window as a promising candidate for optical gain media.

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

Environmental Qualification of a Single-Crystal Silicon Mirror for Spaceflight Use

NASA Technical Reports Server (NTRS)

Hagopian, John; Chambers, John; Rohrback. Scott; Bly, Vincent; Morell, Armando; Budinoff, Jason

2013-01-01

This innovation is the environmental qualification of a single-crystal silicon mirror for spaceflight use. The single-crystal silicon mirror technology is a previous innovation, but until now, a mirror of this type has not been qualified for spaceflight use. The qualification steps included mounting, gravity change measurements, vibration testing, vibration- induced change measurements, thermal cycling, and testing at the cold operational temperature of 225 K. Typical mirrors used for cold applications for spaceflight instruments include aluminum, beryllium, glasses, and glass-like ceramics. These materials show less than ideal behavior after cooldown. Single-crystal silicon has been demonstrated to have the smallest change due to temperature change, but has not been spaceflight-qualified for use. The advantage of using a silicon substrate is with temperature stability, since it is formed from a stress-free single crystal. This has been shown in previous testing. Mounting and environmental qualification have not been shown until this testing.

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

NASA Astrophysics Data System (ADS)

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj; Unocic, Raymond R.; Rack, Philip D.; Baddorf, Arthur P.; Ivanov, Ilia N.; Lavrik, Nickolay V.; List, Frederick; Gupta, Nitant; Bets, Ksenia V.; Yakobson, Boris I.; Smirnov, Sergei N.

2018-03-01

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice1 in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection2 approach, which is now realized in 2D geometry. The method relies on `self-selection' of the fastest-growing domain orientation, which eventually overwhelms the slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h-1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.

Bulk growth of <001> organic nonlinear optical (NLO) L-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals by SR method

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

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

2015-06-24

A transparent uniaxial L-arginine 4-nitrophenolate 4-nitrophenol dehydrate (LAPP) single crystal having dimension of 20 mm diameter and 45 mm length was grown by Sankaranarayanan-Ramasamy (SR) method with a growth rate of 1 mm per day. Using an identical solution the conventional crystal grown to a dimension of 8×5×5 mm{sup 3} was obtained over a period of 30 days. The crystal structure has been confirmed by single crystal X-ray diffraction measurement. The crystalline perfection of LAPP crystals grown by slow evaporation solution technique (SEST) and SR method were characterized using Vickers microhardness, UV-Vis NIR, chemical etching, dark and photo current measurements. The above study indicatesmore » that the crystal quality of the Sankaranarayanan-Ramasamy (SR) method grown LAPP is good compared to the conventional method grown crystal.« less

A Novel Method of Fabricating a Well-Faceted Large-Crystal Diamond Through MPCVD

NASA Astrophysics Data System (ADS)

Man, Weidong; Weng, Jun; Wu, Yuqiong; Chen, Peng; Yu, Xuechao; Wang, Jianhua

2009-12-01

A novel method was developed to deposit a large crystal diamond with good facets up to 1000 μm on a tungsten substrate using a microwave plasma enhanced chemical vapor deposition (MPCVD). This method consists of two steps, namely single-crystal nucleation and growth. Prior to the fabrication of the well-faceted, large crystal diamond, an investigation was made into the nucleation and growth of the diamond which were affected by the O2 concentration and substrate temperature. Deposited diamond crystals were characterized by scanning electron microscopy and micro-Raman spectroscopy. The results showed that the conditions of single-crystal nucleation were appropriate when the ratio of H2/CH4/O2 was about 200/7.0/2.0, while the substrate temperature Ts of 1000°C to 1050°C was the appropriate range for single-crystal diamond growth. Under the optimum parameters, a well-faceted large crystal diamond was obtained.

Fabrication of graded index single crystal in glass

PubMed Central

Veenhuizen, Keith; McAnany, Sean; Nolan, Daniel; Aitken, Bruce; Dierolf, Volkmar; Jain, Himanshu

2017-01-01

Lithium niobate crystals were grown in 3D through localized heating by femtosecond laser irradiation deep inside 35Li2O-35Nb2O5-30SiO2 glass. Laser scanning speed and power density were systematically varied to control the crystal growth process and determine the optimal conditions for the formation of single crystal lines. EBSD measurements showed that, in principle, single crystals can be grown to unlimited lengths using optimal parameters. We successfully tuned the parameters to a growth mode where nucleation and growth occur upon heating and ahead of the scanning laser focus. This growth mode eliminates the problem reported in previous works of non-uniform polycrystallinity because of a separate growth mode where crystallization occurs during cooling behind the scanning laser focus. To our knowledge, this is the first report of such a growth mode using a fs laser. The crystal cross-sections possessed a symmetric, smooth lattice misorientation with respect to the c-axis orientation in the center of the crystal. Calculations indicate the observed misorientation leads to a decrease in the refractive index of the crystal line from the center moving outwards, opening the possibility to produce within glass a graded refractive index single crystal (GRISC) optically active waveguide. PMID:28287174

Thermal, mechanical, optical and dielectric properties of piperazinium hydrogen phosphite monohydrate NLO single crystal

NASA Astrophysics Data System (ADS)

Rajkumar, R.; Praveen Kumar, P.

2018-05-01

Optical transparent crystal of piperazinium hydrogen phosphite monohydrate (PHPM) was grown by slow evaporation method. The grown crystal was characterized by single crystal X-ray diffraction analysis and the crystal belongs to monoclinic system. The functional groups present in PHPM crystal were confirmed by FTIR analysis. UV-Visible spectrum shows that the PHPM crystal is transparent in the visible region. The mechanical behavior of PHPM crystal was characterized by Vickers hardness test. Thermal stability of PHPM crystal was analyzed by thermogravimetric analysis. Dielectric studies were also carried out for the grown crystal. The third-order nonlinear parameters such as nonlinear refractive index and nonlinear absorption coefficient have been calculated using Z scan technique.

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.

Single crystal fibers for high power lasers

NASA Astrophysics Data System (ADS)

Kim, W.; Florea, C.; Baker, C.; Gibson, D.; Shaw, L. B.; Bowman, S.; O'Connor, S.; Villalobos, G.; Bayya, S.; Aggarwal, I. D.; Sanghera, J. S.

2012-11-01

In this paper, we present our recent results in developing cladded-single crystal fibers for high power single frequency fiber lasers significantly exceeding the capabilities of existing silica fiber based lasers. This fiber laser would not only exploit the advantages of crystals, namely their high temperature stability, high thermal conductivity, superior environmental ruggedness, high propensity for rare earth ion doping and low nonlinearity, but will also provide the benefits from an optical fiber geometry to enable better thermal management thereby enabling the potential for high laser power output in short lengths. Single crystal fiber cores with diameters as small as 35μm have been drawn using high purity rare earth doped ceramic or single crystal feed rods by Laser Heated Pedestal Growth (LHPG) process. The mechanical, optical and morphological properties of these fibers have been characterized. The fibers are very flexible and show good overall uniformity. We also measured the optical loss as well as the non-radiative loss of the doped crystal fibers and the results show that the fibers have excellent optical and morphological quality. The gain coefficient of the crystal fiber matches the low quantum defect laser model and it is a good indication of the high quality of the fibers.

Electromagnetic induction heating for single crystal graphene growth: morphology control by rapid heating and quenching

NASA Astrophysics Data System (ADS)

Wu, Chaoxing; Li, Fushan; Chen, Wei; Veeramalai, Chandrasekar Perumal; Ooi, Poh Choon; Guo, Tailiang

2015-03-01

The direct observation of single crystal graphene growth and its shape evolution is of fundamental importance to the understanding of graphene growth physicochemical mechanisms and the achievement of wafer-scale single crystalline graphene. Here we demonstrate the controlled formation of single crystal graphene with varying shapes, and directly observe the shape evolution of single crystal graphene by developing a localized-heating and rapid-quenching chemical vapor deposition (CVD) system based on electromagnetic induction heating. Importantly, rational control of circular, hexagonal, and dendritic single crystalline graphene domains can be readily obtained for the first time by changing the growth condition. Systematic studies suggest that the graphene nucleation only occurs during the initial stage, while the domain density is independent of the growth temperatures due to the surface-limiting effect. In addition, the direct observation of graphene domain shape evolution is employed for the identification of competing growth mechanisms including diffusion-limited, attachment-limited, and detachment-limited processes. Our study not only provides a novel method for morphology-controlled graphene synthesis, but also offers fundamental insights into the kinetics of single crystal graphene growth.

Rotating lattice single crystal architecture on the surface of glass

DOE PAGES

Savytskii, D.; Jain, H.; Tamura, N.; ...

2016-11-03

Defying the requirements of translational periodicity in 3D, rotation of the lattice orientation within an otherwise single crystal provides a new form of solid. Such rotating lattice single (RLS) crystals are found, but only as spherulitic grains too small for systematic characterization or practical application. Here we report a novel approach to fabricate RLS crystal lines and 2D layers of unlimited dimensions via a recently discovered solid-to-solid conversion process using a laser to heat a glass to its crystallization temperature but keeping it below the melting temperature. The proof-of-concept including key characteristics of RLS crystals is demonstrated using the examplemore » of Sb 2S 3 crystals within the Sb-S-I model glass system for which the rotation rate depends on the direction of laser scanning relative to the orientation of initially formed seed. Lattice rotation in this new mode of crystal growth occurs upon crystallization through a well-organized dislocation/disclination structure introduced at the glass/ crystal interface. Implications of RLS growth on biomineralization and spherulitic crystal growth are noted.« less

Top-seeded solution growth and morphology change of RbTiOPO4:Ta single crystal

NASA Astrophysics Data System (ADS)

Li, Ziqing; Chen, Yang; Zhu, Pengfei; Ji, Nianjing; Duan, Xiulan; Jiang, Huaidong

2018-04-01

The RbTiOPO4:Ta single crystal with dimensions of 4 mm × 31 mm × 18 mm was successfully grown by Top Seeded Solution Growth Technique. It is concluded that the doping Ta element can strongly influence the growth and morphology of the RbTiOPO4 crystal. The evident morphology change of RbTiOPO4:Ta crystal with respect to RbTiOPO4 crystal has been observed and the (1 0 0) crystal face was more developed than any other crystal faces. The possible reasons of the morphology change were analyzed through experimental and theoretical methods. Several methods were tried to increase crystallographic a direction dimension of RbTiOPO4:Ta crystals. Finally, the RbTiOPO4:Ta single crystal with crystallographic a direction dimension up to 6 mm was obtained by using thicker seed crystal. This way makes it possible to get isometric RbTiOPO4:Ta crystals, which is beneficial for nonlinear optical applications due to larger area in x-y plane.

Single crystal X- and Q-band EPR spectroscopy of a binuclear Mn(2)(III,IV) complex relevant to the oxygen-evolving complex of photosystem II.

PubMed

Yano, Junko; Sauer, Kenneth; Girerd, Jean-Jacques; Yachandra, Vittal K

2004-06-23

The anisotropic g and hyperfine tensors of the Mn di-micro-oxo complex, [Mn(2)(III,IV)O(2)(phen)(4)](PF(6))(3).CH(3)CN, were derived by single-crystal EPR measurements at X- and Q-band frequencies. This is the first simulation of EPR parameters from single-crystal EPR spectra for multinuclear Mn complexes, which are of importance in several metalloenzymes; one of them is the oxygen-evolving complex in photosystem II (PS II). Single-crystal [Mn(2)(III,IV)O(2)(phen)(4)](PF(6))(3).CH(3)CN EPR spectra showed distinct resolved (55)Mn hyperfine lines in all crystal orientations, unlike single-crystal EPR spectra of other Mn(2)(III,IV) di-micro-oxo bridged complexes. We measured the EPR spectra in the crystal ab- and bc-planes, and from these spectra we obtained the EPR spectra of the complex along the unique a-, b-, and c-axes of the crystal. The crystal orientation was determined by X-ray diffraction and single-crystal EXAFS (Extended X-ray Absorption Fine Structure) measurements. In this complex, the three crystallographic axes, a, b, and c, are parallel or nearly parallel to the principal molecular axes of Mn(2)(III,IV)O(2)(phen)(4) as shown in the crystallographic data by Stebler et al. (Inorg. Chem. 1986, 25, 4743). This direct relation together with the resolved hyperfine lines significantly simplified the simulation of single-crystal spectra in the three principal directions due to the reduction of free parameters and, thus, allowed us to define the magnetic g and A tensors of the molecule with a high degree of reliability. These parameters were subsequently used to generate the solution EPR spectra at both X- and Q-bands with excellent agreement. The anisotropic g and hyperfine tensors determined by the simulation of the X- and Q-band single-crystal and solution EPR spectra are as follows: g(x) = 1.9887, g(y) = 1.9957, g(z) = 1.9775, and hyperfine coupling constants are A(III)(x) = |171| G, A(III)(y) = |176| G, A(III)(z) = |129| G, A(IV)(x) = |77| G, A(IV)(y) = |74| G, A(IV)(z) = |80| G.

Basic and Applied Research in the Field of Electronics and Communications.

DTIC Science & Technology

1986-03-19

301 Theses ?9. N. P. Vlannes, "Optical and :nduction Probing of aSagnezos:atic -vaves in Thin Films of Yttrium :ron Garnet ," ?H D Thesis, Departrment f...used in high-quality, single-crystal ferrite thin films . Both experimental and theoretical analyses verified several new transmission modes, and...4-amD :urrent at 160 kilohertz. (References: 52, 61, 134). X’NM. Control of Microstructure in Thin- Film Electronic Materials Professor C. Thompson

Perovskite single crystals and thin films for optoelectronic devices (Conference Presentation)

NASA Astrophysics Data System (ADS)

Li, Gang; Han, Qifeng; Yang, Yang; Bae, Sang-Hoon; Sun, Pengyu

2016-09-01

Hybrid organolead trihalide perovskite (OTP) solar cells have developed as a promising candidate in photovoltaics due to their excellent properties including a direct bandgap, strong absorption coefficient, long carrier lifetime, and high mobility. Most recently, formamidinium (NH2CH=NH2+ or FA) lead iodide (FAPbI3) has attracted significant attention due to several advantages: (1) the larger organic FA cation can replace the MA cation and form a more symmetric crystal structure, (2) the smaller bandgap of FAPbI3 allows for near infrared (NIR) absorption, and (3) FAPbI3 has an elevated decomposition temperature and thus potential to improve stability. Single crystals provide an excellent model system to study the intrinsic electrical and optical properties of these materials due to their high purity, which is particularly important to understand the limits of these materials. In this work, we report the growth of large ( 5 millimeter size) single crystal FAPbI3 using a novel liquid based crystallization method. The single crystal FAPbI3 demonstrated a δ-phase to α-phase transition with a color change from yellow to black when heated to 185°C within approximately two minutes. The crystal structures of the two phases were identified and the PL emission peak of the α-phase FAPbI3 (820 nm) shows clear red-shift compared to the FAPbI3 thin film (805 nm). The FAPbI3 single crystal shows a long carrier lifetime of 484 ns, a high carrier mobility of 4.4 cm2·V-1·s-1, and even more interestingly a conductivity of 1.1 × 10-7(ohm·cm)-1, which is approximately one order of magnitude higher than that of the MAPbI3 single crystal. Finally, high performance photoconductivity type photodetectors were successfully demonstrated using the single crystal FAPbI3.

Synthesis, crystal structure, spectroscopic characterization, docking simulation and density functional studies of 1-(3,4-dimethoxyphenyl) -3-(4-flurophenyl)-propan-1-one

NASA Astrophysics Data System (ADS)

Khamees, Hussien Ahmed; Jyothi, Mahima; Khanum, Shaukath Ara; Madegowda, Mahendra

2018-06-01

The compound 1-(3,4-dimethoxyphenyl)-3-(4-flurophenyl)-propan-1-one (DFPO) was synthesized by Claisen-Schmidt condensation reaction and the single crystals were obtained by slow evaporation method. Three-dimensional structure was confirmed by single crystal X-ray diffraction method and exhibiting the triclinic crystal system with space group P-1. The crystal structure is stabilized by Csbnd H⋯O intermolecular and weak interactions. Computed molecular geometry has been obtained by density functional theory (DFT) and compared with experimental results. The spectra of both FT-IR in the range (4000-400 cm-1) and FT- Raman (3500-50 cm-1) of DFPO were recorded experimentally and computed by (DFT) using B3LYP/6-311G (d,p) as basis sets. Intramolecular charge transfer has been scanned using natural bond orbital (NBO) analysis and revealed the various contribution of bonding and lone pair to the stabilization of molecule. Nonlinear optical activity (NLO) of the title compound has been determined by second harmonic generation (SHG) and computed using DFT method. Hyperpolarizability, HOMO-LUMO energy gap, hardness, softness electronegativity and others Global reactivity descriptors of DFPO has been calculated and revealed complete picture of chemical reactivity of DFPO. Hirshfeld surface analyses were applied to investigate the intermolecular interactions and revealed that more than two-thirds of the inter contacts are associated with O⋯H, C⋯H and H⋯H interactions. Docking studies of DFPO showed inhibition of Vascular endothelial growth Factor human receptor (VEGFR-2) signalling pathway, which indicates DFPO as anti-angiogenesis, that play pivotal role in cancer, so we suggest it for clinical studies to evaluate its potential to treat human cancers.

A study on the magnetic susceptibilities and optical absorption spectra on single crystals of Gd(III) pyrogermanate

NASA Astrophysics Data System (ADS)

Kundu, T.; Ghosh, D.; Wanklyn, B. M.

1990-04-01

The paper reports for the first time the experimental results of the measurements of magnetic susceptibilities ( K⊥ and K|) and their anisotropy (Δ K) between 300 and 21.8 K and the optical absorption spectra (UV region) at 12.5 K on single crystals of gadolinium pyrogermanate (GdPG). The anisotropy, which is only 211×10 -6 emu/mol at room temperature and increases by two orders of magnitude at 21 K, is predominantly a crystal field (CF) effect on the 8S {7}/{2} ground term, through higher order perturbations. Interpretation of the observed magnetic data was carried out by considering a conventional spin Hamiltonian ( Hs) to derive expressions for K⊥ and K| in terms of four effective crystal field parameters (ECFP). The value s of ECFP were varied to obtain a very close fitting between the theoretical and experimental values of K⊥, K|, δ K and K¯ The splitting of the 8S {7}/{2} term corresponding to these values of ECFP was found to be large, which suggests a strong CF effect in GdPG, as also observed in other RPG crystal studied earlier. The thermal characteristics of the magnetic anisotropy below 30 K deviate by about 5% which could not be explained by CF effects alone. A series expansion method was adopted to analyse the results of K⊥ and K| below 30 K, however the corresponding coefficient B2α and B3α were observed t o be unusually high indicating the presence of CF effect even in this temperature region. The Schottky specific heat, Csch, between 300 and 21 K for GdPG has been calculated and this shows a maximum at Tmax=17 K.

5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

NASA Astrophysics Data System (ADS)

Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

2015-07-01

Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

Single crystal micromechanical resonator and fabrication methods thereof

DOEpatents

Olsson, Roy H.; Friedmann, Thomas A.; Homeijer, Sara Jensen; Wiwi, Michael; Hattar, Khalid Mikhiel; Clark, Blythe; Bauer, Todd; Van Deusen, Stuart B.

2016-12-20

The present invention relates to a single crystal micromechanical resonator. In particular, the resonator includes a lithium niobate or lithium tantalate suspended plate. Also provided are improved microfabrication methods of making resonators, which does not rely on complicated wafer bonding, layer fracturing, and mechanical polishing steps. Rather, the methods allow the resonator and its components to be formed from a single crystal.

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.

Critical experiments of the self-consistent model for polycrystalline Hastelloy-X

NASA Technical Reports Server (NTRS)

Shi, Shixiang; Walker, Kevin P.; Jordan, Eric H.

1991-01-01

A viscoplastic constitutive model is presented for the estimation of the overall mechanical response of Hastelloy-X polycrystalline metals from a knowledge of single crystal behavior. The behavior of polycrystal is derived from that of single crystals using a self-consistent formulation. The single crystal behavior which has been used was developed by summing postulated slip on crystallographic slip systems. The plasticity and creep are treated coupledly using unified viscoplastic model which includes the interaction effects between rapid and slow deformation at elevated temperature. The validity of the model is directly tested by experiments on Hastelloy-X in both single crystal and polycrystalline versions.

High quality factor single-crystal diamond mechanical resonators

NASA Astrophysics Data System (ADS)

Ovartchaiyapong, P.; Pascal, L. M. A.; Myers, B. A.; Lauria, P.; Bleszynski Jayich, A. C.

2012-10-01

Single-crystal diamond is a promising material for microelectromechanical systems (MEMs) because of its low mechanical loss, compatibility with extreme environments, and built-in interface to high-quality spin centers. But its use has been limited by challenges in processing and growth. We demonstrate a wafer bonding-based technique to form diamond on insulator, from which we make single-crystal diamond micromechanical resonators with mechanical quality factors as high as 338 000 at room temperature. Variable temperature measurements down to 10 K reveal a nonmonotonic dependence of quality factor on temperature. These resonators enable integration of single-crystal diamond into MEMs technology for classical and quantum applications.

Effect of Hf-Rich Particles on the Creep Life of a High-strength Nial Single Crystal Alloy

NASA Technical Reports Server (NTRS)

Garg, A.; Raj, S. V.; Darolia, R.

1995-01-01

Additions of small amounts of Hf and Si to NiAl single crystals significantly improve their high-temperature strength and creep properties. However, if large Hf-rich dendritic particles formed during casting of the alloyed single crystals are not dissolved completely during homogenization heat treatment, a large variation in creep rupture life can occur. This behavior, observed in five samples of a Hf containing NiAl single crystal alloy tested at 1144 K under an initial stress of 241.4 MPa, is described in detail highlighting the role of interdendritic Hf-rich particles in limiting creep rupture life.

Ductile-to-Brittle transition in <111> hadfield steel single crystals

NASA Astrophysics Data System (ADS)

Astafurova, E. G.; Chumlyakov, Yu. I.

2010-10-01

The deformation mechanism and the character of fracture of <111> austenitic Hadfield steel single crystals are studied during tension in the temperature range 77-673 K by scanning and transmission electron microscopy. It is found that a change in the fracture mechanism from ductile to brittle fracture according to the fractography criterion takes place at a higher temperature than that determined from a change in the elongation to failure of the single crystals. The ductile-to-brittle transition in the Hadfield steel single crystals is shown to be related to a high level of deforming stresses induced by solid-solution hardening and to mechanical twinning.

Single crystal growth and structural evolution across the 1st order valence transition in (Pr 1–yY y) 1–xCa xCoO 3-δ

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

Schreiber, N. J.; Zhang, Junjie; Zheng, Hong

Here, praseodymium-containing cobalt perovskites, such as (Pr 1-yY y) 1-xCa xCoO 3-δ, have been argued to undergo a first-order charge shift between Pr and hybridized Co-O orbitals that leads to a metal-insulator transition at a temperature, T VT. Magnetization and x-ray absorption spectroscopy measurements on single crystals of (Pr 0.85Y 0.15) 0.7Ca 0.3CoO 3-δ grown in an IR image furnace under 40-60 bar of oxygen confirm the presence of this valence transition. Single crystal x-ray synchrotron diffraction measurements are consistent with an isomorphic phase transition at T VT. No evidence of charge ordering was revealed by the single crystal diffraction.more » Dissimilar to analytical transmission electron microscopy measurements performed on a grain from a polycrystalline sample that revealed an oxygen vacancy order-disorder transition at T VT, the present single-crystal measurements did not evidence such a transition, likely reflecting a lower density of oxygen vacancies in the high-pO 2 grown single crystals.« less

Low-cost single-crystal turbine blades, volume 2

NASA Technical Reports Server (NTRS)

Strangman, T. E.; Dennis, R. E.; Heath, B. R.

1984-01-01

The overall objectives of Project 3 were to develop the exothermic casting process to produce uncooled single-crystal (SC) HP turbine blades in MAR-M 247 and higher strength derivative alloys and to validate the materials process and components through extensive mechanical property testing, rig testing, and 200 hours of endurance engine testing. These Program objectives were achieved. The exothermic casting process was successfully developed into a low-cost nonproperietary method for producing single-crystal castings. Single-crystal MAR-M 247 and two derivatives DS alloys developed during this project, NASAIR 100 and SC Alloy 3, were fully characterized through mechanical property testing. SC MAR-M 247 shows no significant improvement in strength over directionally solidified (DS) MAR-M 247, but the derivative alloys, NASAIR 100 and Alloy 3, show significant tensile and fatigue improvements. Firtree testing, holography, and strain-gauge rig testing were used to determine the effects of the anisotropic characteristics of single-crystal materials. No undesirable characteristics were found. In general, the single-crystal material behaved similarly to DS MAR-M 247. Two complete engine sets of SC HP turbine blades were cast using the exothermic casting process and fully machined. These blades were successfully engine-tested.

Single crystal growth and structural evolution across the 1st order valence transition in (Pr 1–yY y) 1–xCa xCoO 3-δ

DOE PAGES

Schreiber, N. J.; Zhang, Junjie; Zheng, Hong; ...

2017-06-27

Here, praseodymium-containing cobalt perovskites, such as (Pr 1-yY y) 1-xCa xCoO 3-δ, have been argued to undergo a first-order charge shift between Pr and hybridized Co-O orbitals that leads to a metal-insulator transition at a temperature, T VT. Magnetization and x-ray absorption spectroscopy measurements on single crystals of (Pr 0.85Y 0.15) 0.7Ca 0.3CoO 3-δ grown in an IR image furnace under 40-60 bar of oxygen confirm the presence of this valence transition. Single crystal x-ray synchrotron diffraction measurements are consistent with an isomorphic phase transition at T VT. No evidence of charge ordering was revealed by the single crystal diffraction.more » Dissimilar to analytical transmission electron microscopy measurements performed on a grain from a polycrystalline sample that revealed an oxygen vacancy order-disorder transition at T VT, the present single-crystal measurements did not evidence such a transition, likely reflecting a lower density of oxygen vacancies in the high-pO 2 grown single crystals.« less

Investigation of crystal growth in zero gravity environment and investigation of metallic whiskers

NASA Technical Reports Server (NTRS)

Davis, J. H.; Lal, R. B.; Walter, H. U.; Castle, J. G., Jr.

1972-01-01

Theoretical and experimental work reported relates to the effects of near-zero gravity on growths of crystals and metallic whiskers during Skylab and Apollo flight experiments. Studies on growth and characterization of candidate materials for flight experiments cover indium-bismuth compounds, bismuth single crystals, gallium arsenide films and single crystals, and cadmium whiskers.

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.

Growth, piezoelectric study and particle size dependent SHG of an 80 mm long SR grown imidazolium l-tartrate single crystals

NASA Astrophysics Data System (ADS)

Jauhar, RO MU; Era, Paavai; Murugakoothan, P.

2018-05-01

Single crystal of imidazolium l-tartrate (IMLT), an organic nonlinear optical material, was successfully grown by slow evaporation solution growth technique (SEST) and Sankaranarayanan - Ramasamy (SR) method. The crystal structure and its lattice parameters were confirmed by single crystal X-ray diffraction study. The IMLT crystal belongs to monoclinic crystal system having a = 7.579(6) Å, b = 6.911(4) Å, c = 8.9281(5) Å, β = 101.45(8)°, volume, V = 458.33 Å3. The d33 coefficient found from the the piezoelectric study is 23 pC/N. The relative second harmonic generation efficiency of IMLT was found to be 3.16 times that of reference KDP material.

Modified floating-zone growth of organic single crystals

NASA Astrophysics Data System (ADS)

Kou, S.; Chen, C. P.

1994-04-01

For organic materials floating-zone crystal growth is superior to other melt growth processes in two significant respects: (1) the absence of crucible-induced mechanical damage and (2) minimum heating-induced chemical degradation. Due to the rather low surface tension of organic melts, however, floating-zone crystal growth under normal gravity has not been possible so far but microgravity is ideal for such a purpose. With the help of a modified floating-zone technique, organic single crystals of small cross-sections were test grown first under normal gravity. These small crystals were round and rectangular single crystals of benzil and salol, up to about 7 cm long and 6 mm in diameter or 9 mm × 3 mm in cross-section.

Electrical resistivity measurements on fragile organic single crystals in the diamond anvil cell

NASA Astrophysics Data System (ADS)

Adachi, T.; Tanaka, H.; Kobayashi, H.; Miyazaki, T.

2001-05-01

A method of sample assembly for four-probe resistivity measurements on fragile organic single crystals using a diamond anvil cell is presented. A procedure to keep insulation between the metal gasket and four leads of thin gold wires bonded to the sample crystal by gold paint is described in detail. The resistivity measurements performed on a single crystal of an organic semiconductor and that of neutral molecules up to 15 GPa and down to 4.2 K showed that this new procedure of four-probe diamond anvil resistivity measurements enables us to obtain sufficiently accurate resistivity data of organic crystals.

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

Zhang, Junjie; Zheng, Hong; Ren, Yang

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

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.

Synthesis, crystal growth and characterization of a phase matchable nonlinear optical single crystal: p-chloro dibenzylideneacetone

NASA Astrophysics Data System (ADS)

Ravindra, H. J.; John Kiran, A.; Nooji, Satheesha Rai; Dharmaprakash, S. M.; Chandrasekharan, K.; Kalluraya, Balakrishna; Rotermund, Fabian

2008-05-01

Good quality single crystals of p-chloro dibenzylideneacetone (CDBA) of size 13 mm×8 mm×2 mm were grown by slow evaporation solution growth technique. The grown crystals were confirmed by elemental analysis, Fourier transform infrared (FTIR) analysis and single crystal X-ray diffraction techniques. From the thermo gravimetric/differential thermal (TG/DT) analysis, the CDBA was found to be thermally stable up to 250 °C. The mechanical stability of the crystal is comparable with that of the other reported chalcones. The lower optical cut-off wavelength for this crystal was observed at 440 nm. The laser damage threshold of the crystal was 0.6 GW/cm 2 at 532 nm. The second harmonic generation conversion efficiency of the powder sample of CDBA was found to be 4.5 times greater than that of urea. We also demonstrate the existence of the phase matching property in this crystal using Kurtz powder technique.

Method for preparing homogeneous single crystal ternary III-V alloys

DOEpatents

Ciszek, Theodore F.

1991-01-01

A method for producing homogeneous, single-crystal III-V ternary alloys of high crystal perfection using a floating crucible system in which the outer crucible holds a ternary alloy of the composition desired to be produced in the crystal and an inner floating crucible having a narrow, melt-passing channel in its bottom wall holds a small quantity of melt of a pseudo-binary liquidus composition that would freeze into the desired crystal composition. The alloy of the floating crucilbe is maintained at a predetermined lower temperature than the alloy of the outer crucible, and a single crystal of the desired homogeneous alloy is pulled out of the floating crucible melt, as melt from the outer crucible flows into a bottom channel of the floating crucible at a rate that corresponds to the rate of growth of the crystal.

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.

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

A finite-strain homogenization model for viscoplastic porous single crystals: II - Applications

NASA Astrophysics Data System (ADS)

Song, Dawei; Ponte Castañeda, P.

2017-10-01

In part I of this work (Song and Ponte Castañeda, 2017a), a new homogenization-based constitutive model was developed for the finite-strain, macroscopic response of porous viscoplastic single crystals. In this second part, the new model is first used to investigate the instantaneous response and the evolution of the microstructure for porous FCC single crystals for a wide range of loading conditions. The loading orientation, Lode angle and stress triaxiality are found to have significant effects on the evolution of porosity and average void shape, which play crucial roles in determining the overall hardening/softening behavior of porous single crystals. The predictions of the model are found to be in fairly good agreement with numerical simulations available from the literature for all loadings considered, especially for low triaxiality conditions. The model is then used to investigate the strong effect of crystal anisotropy on the instantaneous response and the evolution of the microstructure for porous HCP single crystals. For uniaxial tension and compression, the overall hardening/softening behavior of porous HCP crystals is found to be controlled mostly by the evolution of void shape, and not so much by the evolution of porosity. In particular, porous HCP crystals exhibit overall hardening behavior with increasing porosity, while they exhibit overall softening behavior with decreasing porosity. This interesting behavior is consistent with corresponding results for porous FCC crystals, but is found to be more significant for porous HCP crystals with large anisotropy, such as porous ice, where the non-basal slip systems are much harder than the basal systems.

Post-flight analyses of the crystals from the M0003-14 quartz crystal microbalance experiment

NASA Technical Reports Server (NTRS)

Stuckey, W. K.; Radhakrishnan, G.; Wallace, D.

1993-01-01

Quartz Crystal Microbalances constructed by QCM Research were flown on the leading and trailing edges of LDEF as one of the sub-experiments of M0003. Response of the crystals coated with 150 A of In2O3 was recorded during the first 424 days of the mission. A second QCM with crystals coated with 150 A of ZnS was also flown but not monitored. After the flight, the QCM's were disassembled and analyzed in The Aerospace Corporation laboratories. The samples included the crystals from the leading and trailing edge samples of both types of coatings along with the reference crystals, which were inside the QCM housing. Analyses were performed by scanning electron microscopy, energy dispersive x-ray analyses, x-ray photoelectron spectroscopy, ion microprobe mass analysis, and reflectance spectroscopy in the infrared and UV/visible regions. The crystals are contaminated predominantly with silicone compounds. The contamination is higher on the leading edge than on the trailing edge and higher on the exposed crystals than on the reference crystals.

ZnTeO{sub 3} crystal growth by a modified Bridgman technique

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

Nawash, Jalal M., E-mail: nawashj@uww.edu; Lynn, Kelvin G.

2014-12-15

Highlights: • ZnTeO{sub 3} single crystals were grown for the first time by a modified Bridgman method. • The growth is still possible in a system that lacks congruent melting. • A growth is best when melt is exposed to a steeper axial thermal gradient. • Optical and electrical properties were investigated for the grown crystals. - Abstract: Zinc Tellurite (ZnTeO{sub 3}) crystals were grown for the first time using a modified Bridgman method with a 2.5 kHz radio frequency (RF) furnace. Single crystal growth of ZnTeO{sub 3} was hindered by many complicating factors, such as the evaporation of TeO{submore » 2} above 700 °C and the formation of more than one phase during crystal growth. While there were several successful runs that produced ZnTeO{sub 3} single crystals, it was found that large (≥10 cm{sup 3}) single ZnTeO{sub 3} crystals resulted when the crucible was exposed to a steeper vertical thermal gradient and when the temperature of the melt was raised to at least 860 °C. The results of powder X-ray diffraction (XRD) patterns were in accordance with the X-ray powder diffraction file (PDF) for ZnTeO{sub 3}. Some optical, electrical and structural properties of ZnTeO{sub 3} single crystals were reported in this paper.« less

Method for single crystal growth of photovoltaic perovskite material and devices

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

Huang, Jinsong; Dong, Qingfeng

Systems and methods for perovskite single crystal growth include using a low temperature solution process that employs a temperature gradient in a perovskite solution in a container, also including at least one small perovskite single crystal, and a substrate in the solution upon which substrate a perovskite crystal nucleates and grows, in part due to the temperature gradient in the solution and in part due to a temperature gradient in the substrate. For example, a top portion of the substrate external to the solution may be cooled.

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.

Life Prediction of Turbine Blade Nickel Base Superalloy Single Crystals.

DTIC Science & Technology

1986-08-01

mechanical properties between single crystals and the DS version of Mar-M200. Soon it was recognized again through the mechanical property - structure ... property achievements demonstrated by screening and simulated engine tests. 1 Single crystals are the results of extensive investigation on the mechanical ...behavior, (especially fatigue and creep) of, and the structure - property correlations in the equiaxed and directionally solidified (DS) nickel-base

All-thiol-stabilized Ag44 and Au12Ag32 nanoparticles with single-crystal structures.

PubMed

Yang, Huayan; Wang, Yu; Huang, Huaqi; Gell, Lars; Lehtovaara, Lauri; Malola, Sami; Häkkinen, Hannu; Zheng, Nanfeng

2013-01-01

Noble metal nanoparticles stabilized by organic ligands are important for applications in assembly, site-specific bioconjugate labelling and sensing, drug delivery and medical therapy, molecular recognition and molecular electronics, and catalysis. Here we report crystal structures and theoretical analysis of three Ag44(SR)30 and three Au12Ag32(SR)30 intermetallic nanoclusters stabilized with fluorinated arylthiols (SR=SPhF, SPhF2 or SPhCF3). The nanocluster forms a Keplerate solid of concentric icosahedral and dodecahedral atom shells, protected by six Ag2(SR)5 units. Positive counterions in the crystal indicate a high negative charge of 4(-) per nanoparticle, and density functional theory calculations explain the stability as an 18-electron superatom shell closure in the metal core. Highly featured optical absorption spectra in the ultraviolet-visible region are analysed using time-dependent density functional perturbation theory. This work forms a basis for further understanding, engineering and controlling of stability as well as electronic and optical properties of these novel nanomaterials.

Study of the possibility of growing germanium single crystals under low temperature gradients

NASA Astrophysics Data System (ADS)

Moskovskih, V. A.; Kasimkin, P. V.; Shlegel, V. N.; Vasiliev, Y. V.; Gridchin, V. A.; Podkopaev, O. I.; Zhdankov, V. N.

2014-03-01

The possibility of growing germanium single crystals under low temperature gradients in order to produce a dislocation-free material has been studied. Germanium crystals with a dislocation density of about 100-200 cm-2 have been grown in a system with a weight control of crystal growth at maximum axial gradients of about 1.5 K/cm.

Intrinsic Josephson junctions in mesas and ultrathin BSCCO single crystals: Ultimate control of shape and dimensions

NASA Astrophysics Data System (ADS)

Yurgens, A.; You, L. X.; Torstensson, M.; Winkler, D.

2007-09-01

We describe experiments which are only possible through an ultimate control of sample shape and dimensions down to nanometer scale whereby transport measurements can be done in various restricted geometries. We use photolithography patterning together with a flip-chip technique to isolate very thin (d ∼ 100 nm) pieces of Bi2Sr2CaCu2O8+δ (BSCCO) single crystals. Ar-ion milling allows us to further thin these crystals down to a few nanometers in a controlled way. With decreasing thickness below two to three unit cells, the superconducting transition temperature gradually decreases to zero and the in-plane resistivity increases to large values indicating the existence of a superconductor-insulator transition in these ultrathin single crystals. In a refined technique, a precise control of the etching depth from both sides of the crystal makes it possible to form stacks of intrinsic Josephson junctions (IJJs) inside the ultrathin single crystals. The stacks can be tailor-made to any microscopic height (0-9 nm < d), i.e. enclosing a specific number of IJJs (0-6). In certain geometries, by feeding current into the topmost Cu2O4-layer of a mesa on the surface of a BSCCO single crystal, we measured the critical value of this current by detecting a sharp upturn or break in the current-voltage characteristics. From this, we estimate the sheet critical current density of a single Cu2O4 plane to be ∼0.3-0.7 A/cm at 4.5 K, corresponding to a bulk current density of ∼2-5 MA/cm2. These values are among the largest ever reported for BSCCO single crystals, thin-films and tapes.

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.

Bridgman growth and scintillation properties of calcium tungstate single crystal

NASA Astrophysics Data System (ADS)

Wang, Zhenhai; Jiang, Linwen; Chen, Yaping; Chen, Peng; Chen, Hongbing; Mao, Rihua

2017-12-01

CaWO4 single crystal with large size was grown by Bridgman method. The results of transmission spectra show that the transmittance of CaWO4 crystal reaches 79-85% in 320-800 nm wavelength range. The refraction index is near 1.80 in visible and infrared region. CaWO4 crystal shows a broad emission band centered at 424 nm under X-ray excitation and centered at 416 nm under ultraviolet (λex = 280 nm) excitation. The decay kinetics of CaWO4 single crystal shows double-exponential decay with fast decay constant τ1 = 5.4 μs and slow decay constant τ2 = 177.1 μs. The energy resolution of CaWO4 crystal was found to be 31.6% in the net peak of 545.9 channel. Meanwhile, the absolute output is at the lever of 19,000 ± 1000 photons/MeV. The results indicate the scintillator of CaWO4 single crystal has great potential in the applications of high-energy physics and nuclear physics due to its high light output and great energy resolution.

Single crystal growth of submillimeter diameter sapphire tube by the micro-pulling down method

NASA Astrophysics Data System (ADS)

Kamada, Kei; Murakami, Rikito; Kochurikhin, Vladimir V.; Luidmila, Gushchina; Jin Kim, Kyoung; Shoji, Yasuhiro; Yamaji, Akihiro; Kurosawa, Shunsuke; Ohashi, Yuji; Yokota, Yuui; Yoshikawa, Akira

2018-06-01

This paper addresses several aspects of the μ-PD growth technology as applied to submillimeter diameter sapphire tubes for UFD application. The μ-PD method has been successfully adapted for single crystal sapphire tube growth. A compound crucible made possible the growth of single crystal sapphire tube as small as around 0.70-0.72 mm in outer diameter and 0.28-0.29 in inner diameter over 160 mm in length at growth rate of 2-4 mm/min along 〈0 0 1〉 direction. An Ir crucible with a die composed of an equivalent hole and Ir wire was heated by RF coil in N2 atmosphere. The μ-PD method has been successfully adapted for single crystal sapphire tube growth. Grown crystal tube showed good XRC value of 30.2 arcsec.

Anisotropic constitutive modeling for nickel-base single crystal superalloys. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Sheh, Michael Y.

1988-01-01

An anisotropic constitutive model was developed based on crystallographic slip theory for nickel base single crystal superalloys. The constitutive equations developed utilizes drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments were conducted to evaluate the existence of back stress in single crystal superalloy Rene N4 at 982 C. The results suggest that: (1) the back stress is orientation dependent; and (2) the back stress state variable is required for the current model to predict material anelastic recovery behavior. The model was evaluated for its predictive capability on single crystal material behavior including orientation dependent stress-strain response, tension/compression asymmetry, strain rate sensitivity, anelastic recovery behavior, cyclic hardening and softening, stress relaxation, creep and associated crystal lattice rotation. Limitation and future development needs are discussed.

Purification, crystal growth and characterization of CdSe single crystals

NASA Astrophysics Data System (ADS)

Burger, A.; Henderson, D. O.; Morgan, S. H.; Silberman, E.

1991-02-01

CdSe single crystals have been grown from the stoichiometric melt and from Se rich solutions. Here we report the first mid and far infrared spectra of CdSe crystals free of any known impurity bands. Previous studies of the lattice vibrational properties of CdSe crystals have shown the presence of two bands at 538 and 270 cm -1. Modifications in the purification and crystal growth conditions lead us to assign these two bands to a sulfur impurity. Low temperature photoluminescence spectra are also presented and discussed.

Synthesis and crystal structure of a novel Mn(II) coordination polymer with 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxyphenyl)-1-phenylprop-2-en-1-one ligands

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

Wang, G.-F., E-mail: wgf1979@126.com; Zhang, X., E-mail: zhangx@hit.edu.cn; Sun, S.-W., E-mail: s-shuwen@163.com

3-(4-(1H-Benzo[d]imidazol-1-yl)-4-methoxyphenyl)-1-phenylprop-2-en-1-one (L{sup 1}, 1) and its Mn(II) complex, [Mn(L{sup 1}){sub 2}(SCN){sub 2}]{sub ∞} (2), were synthesized and characterized by elemental analyses, IR spectroscopy and single-crystal X-ray diffraction. The Mn(II) ion in 2 is six-coordinated to four nitrogen atoms of two L{sup 1} ligands, two SCN-ligands, and two oxygen atoms of other two L{sup 1} ligands to form a distorted octahedral geometry. Therefore, each L{sup 1} links Mn ions through the O and N atoms to generate 2D sheet structure.

Superposition-model analysis of rare-earth doped BaY2F8

NASA Astrophysics Data System (ADS)

Magnani, N.; Amoretti, G.; Baraldi, A.; Capelletti, R.

The energy level schemes of four rare-earth dopants (Ce3+ , Nd3+ , Dy3+ , and Er3+) in BaY2 F-8 , as determined by optical absorption spectra, were fitted with a single-ion Hamiltonian and analysed within Newman's Superposition Model for the crystal field. A unified picture for the four dopants was obtained, by assuming a distortion of the F- ligand cage around the RE site; within the framework of the Superposition Model, this distortion is found to have a marked anisotropic behaviour for heavy rare earths, while it turns into an isotropic expansion of the nearest-neighbours polyhedron for light rare earths. It is also inferred that the substituting ion may occupy an off-center position with respect to the original Y3+ site in the crystal.

High geomagnetic intensity during the mid-Cretaceous from Thellier analyses of single plagioclase crystals.

PubMed

Tarduno, J A; Cottrell, R D; Smirnov, A V

2001-03-02

Recent numerical simulations have yielded the most efficient geodynamo, having the largest dipole intensity when reversal frequency is low. Reliable paleointensity data are limited but heretofore have suggested that reversal frequency and paleointensity are decoupled. We report data from 56 Thellier-Thellier experiments on plagioclase crystals separated from basalts of the Rajmahal Traps (113 to 116 million years old) of India that formed during the Cretaceous Normal Polarity Superchron. These data suggest a time-averaged paleomagnetic dipole moment of 12.5 +/- 1.4 x 10(22) amperes per square meter, three times greater than mean Cenozoic and Early Cretaceous-Late Jurassic dipole moments when geomagnetic reversals were frequent. This result supports a correlation between intervals of low reversal frequency and high geomagnetic field strength.

Synthesis, spectroscopic characterization and structural investigations of new adduct compound of carbazole with picric acid: DNA binding and antimicrobial studies

NASA Astrophysics Data System (ADS)

Saravanabhavan, Munusamy; Sathya, Krishnan; Puranik, Vedavati G.; Sekar, Marimuthu

2014-01-01

Carbazole picrate (CP), a new organic compound has been synthesized, characterized by various analytical and spectroscopic technique such as FT-IR, UV-Vis, 1H and 13C NMR spectroscopy. An orthorhombic geometry was proposed based on single crystal XRD study. The thermal stability of the crystal was studied by using thermo-gravimetric and differential thermal analyses and found that it was stable up to 170 °C. Further, the newly synthesized title compound was tested for its in vitro antibacterial and antifungal activity against various bacterial and fungal species. Also, the compound was tested for its binding activity with Calf thymus (CT) DNA and the results show a considerable interaction between CP and CT-DNA.

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.

Large piezoelectric properties in KNN-based lead-free single crystals grown by a seed-free solid-state crystal growth method

NASA Astrophysics Data System (ADS)

Yang, Jie; Zhang, Faqiang; Yang, Qunbao; Liu, Zhifu; Li, Yongxiang; Liu, Yun; Zhang, Qiming

2016-05-01

We report lead-free single crystals with a nominal formula of (K0.45Na0.55)0.96Li0.04NbO3 grown using a simple low-cost seed-free solid-state crystal growth method (SFSSCG). The crystals thus prepared can reach maximum dimensions of 6 mm × 5 mm × 2 mm and exhibit a large piezoelectric coefficient d33 of 689 pC/N. Moreover, the effective piezoelectric coefficient d33 * , obtained under a unipolar electric field of 30 kV/cm, can reach 967 pm/V. The large piezoelectric response plus the high Curie temperature (TC) of 432 °C indicate that SFSSCG is an effective approach to synthesize high-performance lead-free piezoelectric single crystals.

Determining heterogeneous slip activity on multiple slip systems from single crystal orientation pole figures

DOE PAGES

Pagan, Darren C.; Miller, Matthew P.

2016-09-01

A new experimental method to determine heterogeneity of shear strains associated with crystallographic slip in the bulk of ductile, crystalline materials is outlined. The method quantifies the time resolved evolution of misorientation within plastically deforming crystals using single crystal orientation pole figures (SCPFs) measured in-situ with X-ray diffraction. A multiplicative decomposition of the crystal kinematics is used to interpret the distributions of lattice plane orientation observed on the SCPFs in terms of heterogeneous slip activity (shear strains) on multiple slip systems. Here, to show the method’s utility, the evolution of heterogeneous slip is quantified in a silicon single crystal plasticallymore » deformed at high temperature at multiple load steps, with slip activity in sub-volumes of the crystal analyzed simultaneously.« less

Fabrication of tensile-strained single-crystalline GeSn on transparent substrate by nucleation-controlled liquid-phase crystallization

NASA Astrophysics Data System (ADS)

Oka, Hiroshi; Amamoto, Takashi; Koyama, Masahiro; Imai, Yasuhiko; Kimura, Shigeru; Hosoi, Takuji; Shimura, Takayoshi; Watanabe, Heiji

2017-01-01

We developed a method of forming single-crystalline germanium-tin (GeSn) alloy on transparent substrates that is based on liquid-phase crystallization. By controlling and designing nucleation during the melting growth process, a highly tensile-strained single-crystalline GeSn layer was grown on a quartz substrate without using any crystal-seeds or catalysts. The peak field-effect hole mobility of 423 cm2/V s was obtained for a top-gate single-crystalline GeSn MOSFET on a quartz substrate with a Sn content of 2.6%, indicating excellent crystal quality and mobility enhancement due to Sn incorporation and tensile strain.

Laser-Heated Floating Zone Production of Single-Crystal Fibers

NASA Technical Reports Server (NTRS)

Ritzert, Frank; Westfall, Leonard

1996-01-01

This report describes how a laser-heated floating zone apparatus can be used to investigate single-crystal fibers of various compositions. A feedrod with a stoichiometric composition of high-purity powders was connected to a pedestal and fed into a laser scan where it combined with a single-crystal fiber seed. A molten zone was formed at this junction. As the feedrod was continuously fed into the laser scan, a single-crystal fiber of a prescribed orientation was withdrawn from the melt. The resultant fibers, whose diameters ranged from 100 to 250 gm, could then be evaluated on the basis of their growth behavior, physical properties, mechanical properties, and fiber perfection.

Anisotropic constitutive modeling for nickel base single crystal superalloys using a crystallographic approach

NASA Technical Reports Server (NTRS)

Stouffer, D. C.; Sheh, M. Y.

1988-01-01

A micromechanical model based on crystallographic slip theory was formulated for nickel-base single crystal superalloys. The current equations include both drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments have been conducted to evaluate the effect of back stress in single crystals. The results showed that (1) the back stress is orientation dependent; and (2) the back stress state variable in the inelastic flow equation is necessary for predicting anelastic behavior of the material. The model also demonstrated improved fatigue predictive capability. Model predictions and experimental data are presented for single crystal superalloy Rene N4 at 982 C.

Synthesis, growth and characterization of 3-nitroacetanilide—A new organic nonlinear optical crystal by Bridgman technique

NASA Astrophysics Data System (ADS)

Lenin, M.; Ramasamy, P.

2008-10-01

Single crystals of 3-nitroacetanilide, an organic nonlinear optical material has been grown by the Bridgman-Stockbarger method. The single crystal X-ray diffraction (XRD) data revealed the noncentrosymmetric crystal structure, which is an essential criterion for second harmonic generation. The crystalline nature of the grown crystals was confirmed using powder XRD techniques. The functional group of the compound is identified by FTIR spectrum. The thermal stability and its tendency to grow as single crystal in solution and in melt have been identified for the new title compound. The UV-vis spectrum of mNAA shows the lower optical cut off at 400 nm and was transparent in the visible region. The second harmonic generation efficiency was found using Kurtz powder technique. The dielectric constant and dielectric loss of the crystal were measured as a function of frequency and temperature, and the results are discussed.

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).

Solution Growth of a Novel Nonlinear Optical Material: L-Histidine Tetrafluoroborate

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Choi, J.; Wang, W. S.; Bhat, K.; Lal, R. B.; Shields, Angela D.; Penn, Benjamin G.; Frazier, Donald O.

1998-01-01

Single crystals of L-Histidine tetrafluoroborate (L-HFB), a semiorganic nonlinear optical (NLO) material have been successfully grown by the temperature lowering and evaporation methods in our laboratory. Solubility curves of L-HFB have been determined in different solvents, such as water, ethanol and acetone. The solubility of L-HFB is very low in acetone, and ethanol, therefore, it is not feasible to grow L-HFB single crystals using these solvents. Good quality single crystals of a novel nonlinear optical material L-HFB have been grown from aqueous solution. Effects of seed orientation on morphologies of L-HFB crystals were studied. The advantages and disadvantage of both the evaporation and the temperature lowering techniques are compared. The single crystals in size 20 x 20 x 10 cubic mm were grown with deionized water as solvent in two weeks with an approximate growth rate of 1.4mm/day. The transmission range for these crystals has been found to be from 250 nm to 1500 nm.

Self-Aligned Growth of Organic Semiconductor Single Crystals by Electric Field.

PubMed

Kotsuki, Kenji; Obata, Seiji; Saiki, Koichiro

2016-01-19

We proposed a novel but facile method for growing organic semiconductor single-crystals via solvent vapor annealing (SVA) under electric field. In the conventional SVA growth process, nuclei of crystals appeared anywhere on the substrate and their crystallographic axes were randomly distributed. We applied electric field during the SVA growth of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) on the SiO2/Si substrate on which a pair of electrodes had been deposited beforehand. Real-time observation of the SVA process revealed that rodlike single crystals grew with their long axes parallel to the electric field and bridged the prepatterned electrodes. As a result, C8-BTBT crystals automatically formed a field effect transistor (FET) structure and the mobility reached 1.9 cm(2)/(V s). Electric-field-assisted SVA proved a promising method for constructing high-mobility single-crystal FETs at the desired position by a low-cost solution process.

Ferromagnetism in CVT grown tungsten diselenide single crystals with nickel doping

NASA Astrophysics Data System (ADS)

Habib, Muhammad; Muhammad, Zahir; Khan, Rashid; Wu, Chuanqiang; Rehman, Zia ur; Zhou, Yu; Liu, Hengjie; Song, Li

2018-03-01

Two dimensional (2D) single crystal layered transition materials have had extensive consideration owing to their interesting magnetic properties, originating from their lattices and strong spin-orbit coupling, which make them of vital importance for spintronic applications. Herein, we present synthesis of a highly crystalline tungsten diselenide layered single crystal grown by chemical vapor transport technique and doped with nickel (Ni) to tailor its magnetic properties. The pristine WSe2 single crystal and Ni-doped crystal were characterized and analyzed for magnetic properties using both experimental and computational aspects. It was found that the magnetic behavior of the 2D layered WSe2 crystal changed from diamagnetic to ferromagnetic after Ni-doping at all tested temperatures. Moreover, first principle density functional theory (DFT) calculations further confirmed the origin of room temperature ferromagnetism of Ni-doped WSe2, where the d-orbitals of the doped Ni atom promoted the spin moment and thus largely contributed to the magnetism change in the 2D layered material.

Structural and spectroscopic investigation of glycinium oxalurate

NASA Astrophysics Data System (ADS)

Kavitha, T.; Pasupathi, G.; Marchewka, M. K.; Anbalagan, G.; Kanagathara, N.

2017-09-01

Glycinium oxalurate (GO) single crystals has been synthesized and grown by the slow solvent evaporation method at room temperature. Single crystal X-ray diffraction study confirms that GO crystal crystallizes in the monoclinic system with centrosymmetric space group P121/c1. The grown crystals are built up from single protonated glycinium residues and single dissociated oxalurate anions. A combination of ionic and donor-acceptor hydrogen-bond interactions linking together the glycine and oxaluric acid residues forms a three-dimensional network. Hydrogen bonded network present in the crystal gives notable vibrational effect. The molecular geometry, vibrational frequencies and intensity of the vibrational bands have been interpreted with the aid of structure optimization based on HF and density functional theory B3LYP methods with 6-311++G(d,p) basis set. Frontier molecular orbital energies and other related electronic properties are calculated. The natural bonding orbital (NBO) charges have been calculated and interpreted. The molecular electrostatic potential map has been constructed and discussed in detail.

Method for harvesting rare earth barium copper oxide single crystals

DOEpatents

Todt, V.R.; Sengupta, S.; Shi, D.

1996-04-02

A method of preparing high temperature superconductor single crystals is disclosed. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid. 2 figs.

Method for harvesting rare earth barium copper oxide single crystals

DOEpatents

Todt, Volker R.; Sengupta, Suvankar; Shi, Donglu

1996-01-01

A method of preparing high temperature superconductor single crystals. The method of preparation involves preparing precursor materials of a particular composition, heating the precursor material to achieve a peritectic mixture of peritectic liquid and crystals of the high temperature superconductor, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals of the high temperature superconductor on the porous substrate. Alternatively, the peritectic mixture can be cooled to a solid mass and reheated on a porous, inert substrate to melt the matrix of peritectic fluid while leaving the crystals melted, allowing the wicking away of the peritectic liquid.

Optical parameters and dispersion behavior of potassium magnesium chloride sulfate single crystals doped with Co+2 ions

NASA Astrophysics Data System (ADS)

Abu El-Fadl, A.; Abd-Elsalam, A. M.

2018-05-01

Single crystals of potassium magnesium chloride sulfate (KMCS) doped with cobalt ions were grown by slow cooling method. Powder XRD study confirmed the monoclinic structure of the grown crystals. The functional group vibrations were checked through FTIR spectroscopy measurements. In optical studies, the absorbance behavior of the crystals and their optical energy gap were established by Tauc plot. The refractive index, the extinction coefficient and other optical constants were calculated for the grown crystals. The normal dispersion of the refractive index was analyzed according to single oscillator Sellmeier's model. The Urbach's rule was applied to analyze the localized states density in the forbidden gap.

Floating zone growth of α-Na 0.90MnO 2 single crystals

DOE PAGES

Dally, Rebecca; Clement, Raphaele J.; Chisnell, Robin; ...

2016-12-03

Here, single crystal growth of α-Na xMnO 2 (x=0.90) is reported via the floating zone technique. The conditions required for stable growth and intergrowth-free crystals are described along with the results of trials under alternate growth atmospheres. Chemical and structural characterizations of the resulting α-Na 0.90MnO 2 crystals are performed using ICP-AES NMR, XANES, XPS, and neutron diffraction measurements. As a layered transition metal oxide with large ionic mobility and strong correlation effects, α-Na xMnO 2 is of interest to many communities, and the implications of large volume, high purity, single crystal growth are discussed.

Energy-dispersive neutron imaging and diffraction of magnetically driven twins in a Ni2MnGa single crystal magnetic shape memory alloy

NASA Astrophysics Data System (ADS)

Kabra, Saurabh; Kelleher, Joe; Kockelmann, Winfried; Gutmann, Matthias; Tremsin, Anton

2016-09-01

Single crystals of a partially twinned magnetic shape memory alloy, Ni2MnGa, were imaged using neutron diffraction and energy-resolved imaging techniques at the ISIS spallation neutron source. Single crystal neutron diffraction showed that the crystal produces two twin variants with a specific crystallographic relationship. Transmission images were captured using a time of flight MCP/Timepix neutron counting detector. The twinned and untwinned regions were clearly distinguishable in images corresponding to narrow-energy transmission images. Further, the spatially-resolved transmission spectra were used to elucidate the orientations of the crystallites in the different volumes of the crystal.

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

DOE PAGES

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj; ...

2018-03-12

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here in this paper we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection approach, which is now realized in 2D geometry. The method relies on ‘self-selection’ of the fastest-growing domain orientation, which eventually overwhelms themore » slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h -1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.« less

Evolutionary selection growth of two-dimensional materials on polycrystalline substrates

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

Vlassiouk, Ivan V.; Stehle, Yijing; Pudasaini, Pushpa Raj

There is a demand for the manufacture of two-dimensional (2D) materials with high-quality single crystals of large size. Usually, epitaxial growth is considered the method of choice in preparing single-crystalline thin films, but it requires single-crystal substrates for deposition. Here in this paper we present a different approach and report the synthesis of single-crystal-like monolayer graphene films on polycrystalline substrates. The technological realization of the proposed method resembles the Czochralski process and is based on the evolutionary selection approach, which is now realized in 2D geometry. The method relies on ‘self-selection’ of the fastest-growing domain orientation, which eventually overwhelms themore » slower-growing domains and yields a single-crystal continuous 2D film. Here we have used it to synthesize foot-long graphene films at rates up to 2.5 cm h -1 that possess the quality of a single crystal. We anticipate that the proposed approach could be readily adopted for the synthesis of other 2D materials and heterostructures.« less

High-Pressure Structural Response of an Insensitive Energetic Crystal: Dihydroxylammonium 5,5'-Bistetrazole-1,1'-diolate (TKX-50)

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

Dreger, Zbigniew A.; Stash, Adam I.; Yu, Zhi-Gang

2017-03-06

The structural response of a novel, insensitive energetic crystal—dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50)—was examined under high pressure. Using synchrotron single-crystal X-ray diffraction measurements, details of molecular, intermolecular, and crystal changes were determined to ~10 GPa to understand its structural stability. The experimental results showed that TKX-50 exhibits highly anisotropic compression and significantly lower volume compressibility than currently known energetic crystals. These results are found to be in general agreement with our previous predictions from the DFT calculations. Additionally, the experimental data revealed anomalous compression—an expansion of the unit cell along the a axis (negative linear compressibility, NLC) upon compression to ~3 GPa.more » The structural analyses demonstrated that this unusual effect, the first such observation in an energetic crystal, is a consequence of the highly anisotropic response of 3D motifs, comprised of two parallel anions [(C 2N 8O 2) 2–] linked with two cations [(NH 3OH) +] through four strong hydrogen bonds. The present results demonstrate that the structural stability of TKX-50 is controlled by the strong and highly anisotropic intermolecular interactions, and these may contribute to its shock insensitivity.« less

High-pressure structural response of an insensitive energetic crystal: Dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50)

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

Dreger, Zbigniew A.; Stash, Adam I.; Yu, Zhi -Gang

The structural response of a novel, insensitive energetic crystal—dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50)—was examined under high pressure. Using synchrotron single-crystal X-ray diffraction measurements, details of molecular, intermolecular, and crystal changes were determined to ~10 GPa to understand its structural stability. The experimental results showed that TKX-50 exhibits highly anisotropic compression and significantly lower volume compressibility than currently known energetic crystals. These results are found to be in general agreement with our previous predictions from the DFT calculations. Additionally, the experimental data revealed anomalous compression—an expansion of the unit cell along the a axis (negative linear compressibility, NLC) upon compression to ~3 GPa.more » The structural analyses demonstrated that this unusual effect, the first such observation in an energetic crystal, is a consequence of the highly anisotropic response of 3D motifs, comprised of two parallel anions [(C 2N 8O 2) 2–] linked with two cations [(NH 3OH) +] through four strong hydrogen bonds. Finally, the present results demonstrate that the structural stability of TKX-50 is controlled by the strong and highly anisotropic intermolecular interactions, and these may contribute to its shock insensitivity.« less

Symbiont-driven sulfur crystal formation in a thiotrophic symbiosis from deep-sea hydrocarbon seeps

PubMed Central

Eichinger, Irmgard; Schmitz-Esser, Stephan; Schmid, Markus; Fisher, Charles R; Bright, Monika

2014-01-01

The siboglinid tubeworm Sclerolinum contortum symbiosis inhabits sulfidic sediments at deep-sea hydrocarbon seeps in the Gulf of Mexico. A single symbiont phylotype in the symbiont-housing organ is inferred from phylogenetic analyses of the 16S ribosomal ribonucleic acid (16S rRNA) gene and fluorescent in situ hybridization. The phylotype we studied here, and a previous study from an arctic hydrocarbon seep population, reveal identical 16S rRNA symbiont gene sequences. While sulfide is apparently the energy source for the symbionts (and ultimately the gutless host), both partners also have to cope with its toxicity. This study demonstrates abundant large sulfur crystals restricted to the trophosome area. Based on Raman microspectroscopy and energy dispersive X-ray analysis, these crystals have the same S8 sulfur configuration as the recently described small sulfur vesicles formed in the symbionts. The crystals reside adjacent to the symbionts in the trophosome. This suggests that their formation is either extra- or intracellular in symbionts. We propose that formation of these crystals provides both energy-storage compounds for the symbionts and serves the symbiosis by removing excess toxic sulfide from host tissues. This symbiont-mediated sulfide detoxification may have been crucial for the establishment of thiotrophic symbiosis and continues to remain an important function of the symbionts. PMID:24992535

High-pressure structural response of an insensitive energetic crystal: Dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50)

DOE PAGES

Dreger, Zbigniew A.; Stash, Adam I.; Yu, Zhi -Gang; ...

2017-02-28

The structural response of a novel, insensitive energetic crystal—dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50)—was examined under high pressure. Using synchrotron single-crystal X-ray diffraction measurements, details of molecular, intermolecular, and crystal changes were determined to ~10 GPa to understand its structural stability. The experimental results showed that TKX-50 exhibits highly anisotropic compression and significantly lower volume compressibility than currently known energetic crystals. These results are found to be in general agreement with our previous predictions from the DFT calculations. Additionally, the experimental data revealed anomalous compression—an expansion of the unit cell along the a axis (negative linear compressibility, NLC) upon compression to ~3 GPa.more » The structural analyses demonstrated that this unusual effect, the first such observation in an energetic crystal, is a consequence of the highly anisotropic response of 3D motifs, comprised of two parallel anions [(C 2N 8O 2) 2–] linked with two cations [(NH 3OH) +] through four strong hydrogen bonds. Finally, the present results demonstrate that the structural stability of TKX-50 is controlled by the strong and highly anisotropic intermolecular interactions, and these may contribute to its shock insensitivity.« less

Synthesis, crystal structure, characterizations and magnetic study of a novel two-dimensional iron fluoride

NASA Astrophysics Data System (ADS)

Bouketaya, Sabrine; Smida, Mouna; Abdelbaky, Mohammed S. M.; Dammak, Mohamed; García-Granda, Santiago

2018-06-01

A new hybrid compound formulated as [Fe3F8(H2O)2](Am2TAZ)2 (Am2TAZ= 3,5-diamino-1,2,4-triazole) was prepared under hydrothermal conditions. The crystal structure was solved by single-crystal X-ray diffraction and the bulk was characterized by thermal analyses (TG-MS), vibrational spectroscopy (FTIR, Raman), Ultraviolet-visible spectroscopy (UV-Vis), and scanning electron microscopy (SEM-EDX). It crystallizes in the triclinic system space group P 1 ̅ with unit cell parameters a= 7.100(2) Å, b= 7.658(2) Å, c= 8.321(2) Å, α = 107.330(20)°, β = 111.842(18)°, γ = 93.049(17)°, Z = 1 and V= 394.01(17) Å3. The studied X-ray crystal structure shows the two oxidation states for iron atoms (Fe2+, Fe3+) and generates a 2D inorganic network, built up of inorganic layers constructed from infinite inorganic chains running along a axis. In fact, these chains are connected via (Fe3+(3)F6) octahedral. OW-H…F and N-H…F hydrogen bonds, making up the whole 3D network, are strongly linked in the layers. Magnetization measurements were performed, exhibiting the paramagnetic feature of the studied compound above 150 K.

Crystallization and preliminary X-ray analysis of binary and ternary complexes of Haloferax mediterranei glucose dehydrogenase

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

Esclapez, Julia; Britton, K. Linda; Baker, Patrick J.

2005-08-01

Single crystals of binary and ternary complexes of wild-type and D38C mutant H. mediterranei glucose dehydrogenase have been obtained by the hanging-drop vapour-diffusion method. Haloferax mediterranei glucose dehydrogenase (EC 1.1.1.47) belongs to the medium-chain alcohol dehydrogenase superfamily and requires zinc for catalysis. In the majority of these family members, the catalytic zinc is tetrahedrally coordinated by the side chains of a cysteine, a histidine, a cysteine or glutamate and a water molecule. In H. mediterranei glucose dehydrogenase, sequence analysis indicates that the zinc coordination is different, with the invariant cysteine replaced by an aspartate residue. In order to analyse themore » significance of this replacement and to contribute to an understanding of the role of the metal ion in catalysis, a range of binary and ternary complexes of the wild-type and a D38C mutant protein have been crystallized. For most of the complexes, crystals belonging to space group I222 were obtained using sodium/potassium citrate as a precipitant. However, for the binary and non-productive ternary complexes with NADPH/Zn, it was necessary to replace the citrate with 2-methyl-2,4-pentanediol. Despite the radical change in conditions, the crystals thus formed were isomorphous.« less

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.

Self-reporting inhibitors: single crystallization process to get two optically pure enantiomers.

PubMed

Wan, Xinhua; Ye, Xichong; Cui, Jiaxi; Li, Bowen; Li, Na; Zhang, Jie

2018-05-22

Collection of two optically pure enantiomers in a single crystallization process can significantly increase the chiral separation efficiency but it's hard to realize nowadays. Herein we describe, for the first time, a self-reporting strategy for visualizing the crystallization process by a kind of dyed self-assembled inhibitors made from the copolymers with tri(ethylene glycol)-grafting polymethylsiloxane as main chains and poly(N6-methacryloyl-L-lysine) as side chains. When applied with seeds together for the fractional crystallization of conglomerates, the inhibitors can label the formation of the secondary crystals and guide us to completely separate the crystallization process of two enantiomers with colorless crystals as the first product and red crystals as the secondary product. This method leads to high optical purity of D/L-Asn·H2O (99.9 ee% for D-crystals and 99.5 ee% for L-crystals) in a single crystallization process. Moreover, it requires low feeding amount of additives and shows excellent recyclability. We foresee its great potential in developing novel chiral separation methods that can be used in different scales. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design and fabrication of PZN-7%PT single crystal high frequency angled needle ultrasound transducers.

PubMed

Zhou, Qifa; Wu, Dawei; Jin, Jing; Hu, Chang-hong; Xu, Xiaochen; Williams, Jay; Cannata, Jonathan M; Lim, Leongchew; Shung, K Kirk

2008-01-01

A high-frequency angled needle ultrasound transducer with an aperture size of 0.4 x 0.56 mm2 was fabricated using a lead zinc niobate-lead titanate (PZN- 7%PT) single crystal as the active piezoelectric material. The single crystal was bonded to a conductive silver particle matching layer and a conductive epoxy backing material through direct contact curing. A parylene outer matching layer was formed by vapor deposition. Angled needle probe configuration was achieved by dicing at 45 degrees to the single crystal poling direction to satisfy a clinical request for blood flow measurement in the posterior portion of the eye. The electrical impedance magnitude and phase of the transducer were 42 Omega and -63 degrees , respectively. The measured center frequency and the fractional bandwidth at -6 dB were 43 MHz and 45%, respectively. The two-way insertion loss was approximately 17 dB. Wire phantom imaging using fabricated PZN-7%PT single crystal transducers was obtained and spatial resolutions were assessed.

Micro-pulling-down furnace modification and single crystal fibers growth

NASA Astrophysics Data System (ADS)

Yuan, Dongsheng; Jia, Zhitai; Li, Yang; Wu, Baiyi; Tao, Xutang

2016-03-01

Single crystal fiber (SCF) combines the excellent instinct properties of conventional bulk laser crystals, and the special geometry advantage of active optical fibers. YAG and LuAG are proper host candidates for single crystal fiber laser with high thermal conductivity. Despite a lower thermal conductivity for pure crystal than YAG, LuAG crystal is easier to obtain homogeneous optical quality, and has a thermal conductivity nearly independent from the doping level. Micropulling- down (μ-PD) has relatively small thermal gradient, and here we use μ-PD to carry out high quality SCFs. Through the μ-PD furnace manufactured by ourselves, crystal fibers with different diameters have been grown successfully. We designed and fabricated a method to adjust the thermal distribution, and with the favor of pulling-down rate, the specific diameter can be controlled perfectly. The crystalline quality and homogeneity along the whole fiber were investigated, and LuAG SCF was confirmed to have a fine crystal quality for laser.

Solid-state microrefrigerator

DOEpatents

Ullom, Joel N.

2003-06-24

A normal-insulator-superconductor (NIS) microrefrigerator in which a superconducting single crystal is both the substrate and the superconducting electrode of the NIS junction. The refrigerator consists of a large ultra-pure superconducting single crystal and a normal metal layer on top of the superconducting crystal, separated by a thin insulating layer. The superconducting crystal can be either cut from bulk material or grown as a thick epitaxial film. The large single superconducting crystal allows quasiparticles created in the superconducting crystal to easily diffuse away from the NIS junction through the lattice structure of the crystal to normal metal traps to prevent the quasiparticles from returning across the NIS junction. In comparison to thin film NIS refrigerators, the invention provides orders of magnitude larger cooling power than thin film microrefrigerators. The superconducting crystal can serve as the superconducting electrode for multiple NIS junctions to provide an array of microrefrigerators. The normal electrode can be extended and supported by microsupports to provide support and cooling of sensors or arrays of sensors.

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

Qiusheng, Y., E-mail: qsyan@gdut.edu.cn; Senkai, C., E-mail: senkite@sina.com; Jisheng, P., E-mail: panjisheng@gdut.edu.cn

Different machining processes were used in the single crystal SiC wafer machining. SEM was used to observe the surface morphology and a cross-sectional cleavages microscopy method was used for subsurface cracks detection. Surface and subsurface cracks characteristics of single crystal SiC wafer in abrasive machining were analysed. The results show that the surface and subsurface cracks system of single crystal SiC wafer in abrasive machining including radial crack, lateral crack and the median crack. In lapping process, material removal is dominated by brittle removal. Lots of chipping pits were found on the lapping surface. With the particle size becomes smaller,more » the surface roughness and subsurface crack depth decreases. When the particle size was changed to 1.5µm, the surface roughness Ra was reduced to 24.0nm and the maximum subsurface crack was 1.2µm. The efficiency of grinding is higher than lapping. Plastic removal can be achieved by changing the process parameters. Material removal was mostly in brittle fracture when grinding with 325# diamond wheel. Plow scratches and chipping pits were found on the ground surface. The surface roughness Ra was 17.7nm and maximum subsurface crack depth was 5.8 µm. When grinding with 8000# diamond wheel, the material removal was in plastic flow. Plastic scratches were found on the surface. A smooth surface of roughness Ra 2.5nm without any subsurface cracks was obtained. Atomic scale removal was possible in cluster magnetorheological finishing with diamond abrasive size of 0.5 µm. A super smooth surface eventually obtained with a roughness of Ra 0.4nm without any subsurface crack.« less

SIKA—the multiplexing cold-neutron triple-axis spectrometer at ANSTO

NASA Astrophysics Data System (ADS)

Wu, C.-M.; Deng, G.; Gardner, J. S.; Vorderwisch, P.; Li, W.-H.; Yano, S.; Peng, J.-C.; Imamovic, E.

2016-10-01

SIKA is a new cold-neutron triple-axis spectrometer receiving neutrons from the cold source CG4 of the 20MW Open Pool Australian Light-water reactor. As a state-of-the-art triple-axis spectrometer, SIKA is equipped with a large double-focusing pyrolytic graphite monochromator, a multiblade pyrolytic graphite analyser and a multi-detector system. In this paper, we present the design, functions, and capabilities of SIKA, and discuss commissioning experimental results from powder and single-crystal samples to demonstrate its performance.

(+)- and (-)-Cajanusine, a pair of new enantiomeric stilbene dimers with a new skeleton from the leaves of Cajanus cajan.

PubMed

Li, Xiao-Long; Zhao, Bing-Xin; Huang, Xiao-Jun; Zhang, Dong-Mei; Jiang, Ren-Wang; Li, Ying-Jie; Jian, Yu-Qing; Wang, Ying; Li, Yao-Lan; Ye, Wen-Cai

2014-01-03

A pair of new enantiomeric stilbene dimers, (+)- and (-)-cajanusine [(+)-1 and (-)-1], with a unique coupling pattern were isolated from the leaves of Cajanus cajan . Their structures including absolute configurations were elucidated on the basis of comprehensive spectroscopic and single-crystal X-ray diffraction analyses, as well as CD calculations. The plausible biogenetic pathway of 1 was also proposed. Additionally, (±)-1, (+)-1, and (-)-1 exhibited inhibitory activities on the growth of human hepatocellular carcinoma cells.

The Fundamentals of Dislocation Transport of Hydrogen in BCC Iron.

DTIC Science & Technology

1984-10-01

4.2.1. Single Crystal Material 24 4.2.2. Polycrystalline Material 25 4.3. Single Crystal Orientation Determination 25 4.4. Straining Permeation Test 27...Test 45 4.6. Supersaturation Study 47 S. RESULTS AND DISCUSSION 50 5.1. Single Crystal Orientation Determination 50 5.1.1. Slip System Determination 58...Orientation 162 Determination B.1. Dislocation Line Direction Determination 162 B.2. Burgers Vector Determination 164

Comparison of the optical parameters of a CaF{sub 2} single crystal and optical ceramics

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

Palashov, O V; Khazanov, E A; Mukhin, I B

Single crystal and optical ceramic CaF{sub 2} samples are studied by the method of thermally induced depolarisation of laser radiation at 1076 nm. The absorption coefficients of the single crystal and ceramics are estimated as {alpha} < 4.5x10{sup -4} cm{sup -1} and {alpha} < 1.33x10{sup -3} cm{sup -1}, respectively. (letters)

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.

Growth and characterization of SrI2:Eu2+ single crystal for gamma ray detector applications

NASA Astrophysics Data System (ADS)

Raja, A.; Daniel, D. Joseph; Ramasamy, P.; Singh, S. G.; Sen, S.; Gadkari, S. C.

2018-04-01

Europium activated Strontium Iodide single crystal was grown by vertical Bridgman-stockbarger technique. The melting point and freezing point of SrI2:Eu2+ crystal was analyzed by TG/DTA. The Radioluminescence emission was recorded. The scintillation measurement was carried out for the grown SrI2:Eu2+ crystal under 137Cs gamma energy source.

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.

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

Kuz'micheva, G. M., E-mail: galkuz@mitht.ru; Zaharko, O.; Tyunina, E. A.

Langatate crystals of the general composition La{sub 3}(Ga{sub 0.5}Ta{sub 0.5})Ga{sub 5}O{sub 14}, grown by the Czochralski method, have been investigated by neutron diffraction (single crystals) and X-ray diffraction (ground single crystals). The crystals were grown in an atmosphere of 99% Ar + 1% O{sub 2} in the Y54{sup o} direction (rotation by 54{sup o} with respect to the y axis), without subsequent annealing (orange crystal) or with vacuum annealing (colorless crystal). It is established that colorless crystals have a higher gallium content and, therefore, a larger number of oxygen vacancies in comparison with colored crystals; this is a possible reasonmore » for their lower microhardness.« less