Science.gov

Sample records for nickel-based single crystal

  1. Anisotropy of nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

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

    1980-01-01

    The effects of crystal orientation on the mechanical properties of single crystals of the nickel-based superalloy Mar-M247 are investigated. Tensile tests at temperatures from 23 to 1093 C and stress rupture tests at temperatures from 760 to 1038 C were performed for 52 single crystals at various orientations. During tensile testing between 23 and 760 C, single crystals with high Schmid factors were found to be favorably oriented for slip and to exhibit lower strength and higher ductility than those with low Schmid factors. Crystals which required large rotations to become oriented for cross slip were observed to have the shortest stress rupture lives at 760 C, while those which required little or no rotation had the longest lives. In addition, stereographic triangles obtained for Mar-M247 and Mar-M200 single crystals reveal that crystals with orientations near the -111 had the highest lives, those near the 001 had high lives, and those near the 011 had low lives.

  2. Bithermal fatigue of a nickel-base superalloy single crystal

    NASA Technical Reports Server (NTRS)

    Verrilli, Michael J.

    1988-01-01

    The thermomechanical fatigue behavior of a nickel-base superalloy single crystal was investigated using a bithermal test technique. The bithermal fatigue test was used as a simple alternative to the more complex thermomechanical fatigue test. Both in-phase and out-of-phase bithermal tests were performed on (100)-oriented coated and bare Rene N4 single crystals. In out-of-plane bithermal tests, the tensile and compressive halves of the cycle were applied isothermally at 760 and 982 C, respectively, while for the in-phase bithermal tests the temperature-loading sequence was reversed. The bithermal fatigue lives of bare specimens were shorter than the isothermal fatigue lives at either temperature extreme when compared on an inelastic strain basis. Both in-phase and out-of-phase bithermal fatigue life curves converged in the large strain regime and diverged in the small strain regime, out-of-phase resulting in the shortest lives. The coating had no effect on life for specimens cycled in-phase; however, the coating was detrimental for isothermal fatigue at 760 C and for out-of-phase fatigue under large strains.

  3. A crystallographic model for nickel base single crystal alloys

    NASA Technical Reports Server (NTRS)

    Dame, L. T.; Stouffer, D. C.

    1988-01-01

    The purpose of this research is to develop a tool for the mechanical analysis of nickel-base single-crystal superalloys, specifically Rene N4, used in gas turbine engine components. This objective is achieved by developing a rate-dependent anisotropic constitutive model and implementing it in a nonlinear three-dimensional finite-element code. The constitutive model is developed from metallurgical concepts utilizing a crystallographic approach. An extension of Schmid's law is combined with the Bodner-Partom equations to model the inelastic tension/compression asymmetry and orientation-dependence in octahedral slip. Schmid's law is used to approximate the inelastic response of the material in cube slip. The constitutive equations model the tensile behavior, creep response and strain-rate sensitivity of the single-crystal superalloys. Methods for deriving the material constants from standard tests are also discussed. The model is implemented in a finite-element code, and the computed and experimental results are compared for several orientations and loading conditions.

  4. Compositional Effects on Nickel-Base Superalloy Single Crystal Microstructures

    NASA Technical Reports Server (NTRS)

    MacKay, Rebecca A.; Gabb, Timothy P.; Garg,Anita; Rogers, Richard B.; Nathal, Michael V.

    2012-01-01

    Fourteen nickel-base superalloy single crystals containing 0 to 5 wt% chromium (Cr), 0 to 11 wt% cobalt (Co), 6 to 12 wt% molybdenum (Mo), 0 to 4 wt% rhenium (Re), and fixed amounts of aluminum (Al) and tantalum (Ta) were examined to determine the effect of bulk composition on basic microstructural parameters, including gamma' solvus, gamma' volume fraction, volume fraction of topologically close-packed (TCP) phases, phase chemistries, and gamma - gamma'. lattice mismatch. Regression models were developed to describe the influence of bulk alloy composition on the microstructural parameters and were compared to predictions by a commercially available software tool that used computational thermodynamics. Co produced the largest change in gamma' solvus over the wide compositional range used in this study, and Mo produced the largest effect on the gamma lattice parameter and the gamma - gamma' lattice mismatch over its compositional range, although Re had a very potent influence on all microstructural parameters investigated. Changing the Cr, Co, Mo, and Re contents in the bulk alloy had a significant impact on their concentrations in the gamma matrix and, to a smaller extent, in the gamma' phase. The gamma phase chemistries exhibited strong temperature dependencies that were influenced by the gamma and gamma' volume fractions. A computational thermodynamic modeling tool significantly underpredicted gamma' solvus temperatures and grossly overpredicted the amount of TCP phase at 982 C. Furthermore, the predictions by the software tool for the gamma - gamma' lattice mismatch were typically of the wrong sign and magnitude, but predictions could be improved if TCP formation was suspended within the software program. However, the statistical regression models provided excellent estimations of the microstructural parameters based on bulk alloy composition, thereby demonstrating their usefulness.

  5. 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.

  6. Characterization of hydrogen embrittlement in nickel base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Chene, J.; Baker, C. L.; Bernstein, I. M.; Williams, J. C.

    1986-01-01

    In order to study the role of CMSX2 single crystal microstructure on the combined stress-hydrogen environment effects, hydrogen was introduced by cathodic charging. Concentration measurements were carried out to investigate the dependence of hydrogen solubility and trapping on microstructure. Mechanical properties were measured at room temperature on smooth tensile specimens as a function of heat treatment, crystal orientation and H charging conditions. SEM and TEM allow to study H induced cracks initiation and propagation. A large amount of hydrogen can be dissolved and trapped in CMSX2 single crystals when exposed to a high hydrogen fugacity environment. The strong H trapping evidenced in voids explains the predominant role of these defects as crack initiation sites. The strong detrimental effect of hydrogen on the material tenacity is discussed.

  7. 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.

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

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Swanson, Gregory R.

    2000-01-01

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

  9. Microstructure-property relationships in directionally solidified single crystal nickel-base superalloys

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.; Nathal, M. V.

    1986-01-01

    Some of the microstructural features which influence the creep properties of directionally solidified and single crystal nickel-base superalloys are discussed. Gamma precipitate size and morphology, gamma-gamma lattice mismatch, phase instability, alloy composition, and processing variations are among the factors considered. Recent experimental results are reviewed and related to the operative deformation mechanisms and to the corresponding mechanical properties. Special emphasis is placed on the creep behavior of single crystal superalloys at high temperatures, where directional gamma coarsening is prominent, and at lower temperatures, where gamma coarsening rates are significantly reduced. It can be seen that very subtle changes in microstructural features can have profound effects on the subsequent properties of these materials.

  10. Behavior of nickel-base superalloy single crystals under thermal-mechanical fatigue

    NASA Astrophysics Data System (ADS)

    Fleury, E.; Rémy, L.

    1994-12-01

    The thermal-mechanical fatigue behavior of AM1 nickel-base superalloy single crystals is studied using a cycle from 600 °C to 1100 °C. It is found to be strongly dependent on crystallo-graphic orientation, which leads to different shapes of the stress-strain hysteresis loops. The cyclic stress-strain response is influenced by variation in Young’s modulus, flow stress, and cyclic hardening with temperature for every crystallographic orientation. The thermalmechanical fatigue life is mainly spent in crack growth. Two main crack-initiation mechanisms occur, depending on the mechanical strain range. Oxidation-induced cracking is the dominant damage mechanism in the lifetime of interest for turbine blades.

  11. Yielding and deformation behavior of the single crystal nickel-base superalloy PWA 1480

    NASA Technical Reports Server (NTRS)

    Milligan, W. W., Jr.

    1986-01-01

    Interrupted tensile tests were conducted to fixed plastic strain levels in 100 ordered single crystals of the nickel based superalloy PWA 1480. Testing was done in the range of 20 to 1093 C, at strain rate of 0.5 and 50%/min. The yield strength was constant from 20 to 760 C, above which the strength dropped rapidly and became a stong function of strain rate. The high temperature data were represented very well by an Arrhenius type equation, which resulted in three distinct temperature regimes. The deformation substructures were grouped in the same three regimes, indicating that there was a fundamental relationship between the deformation mechanisms and activation energies. Models of the yielding process were considered, and it was found that no currently available model was fully applicable to this alloy. It was also demonstrated that the initial deformation mechanism (during yielding) was frequently different from that which would be inferred by examining specimens which were tested to failure.

  12. The high temperature deformation in cyclic loading of a single crystal nickel-base superalloy

    NASA Technical Reports Server (NTRS)

    Gabb, T. P.; Welsch, G.

    1989-01-01

    The high temperature cyclic stress softening response of the single crystal nickel-base superalloy PWA 1480 was investigated. Specimens oriented near the 001- and 111-lines were tested at 1050 C in low-cycle fatigue and then microstructurally evaluated. The 001- and 111-line specimens had dissimilar flow behavior in monotonic tensile tests, but comparable softening in low-cycle fatigue. This softening was accompanied by rapid generation of dislocation networks at the gamma-gamma-prime interfaces and by a slower time-dependent coarsening of gamma-prime precipitates. Due to the rapid formation of a dislocation substructure at the gamma-gamma-prime interfaces, the cyclic stress softening could be modeled with an existing theory which related cyclic stress to the evolving microstructure and dislocation structure.

  13. Effect of crystallographic orientation on plastic deformation of single crystal nickel-base superalloys

    NASA Astrophysics Data System (ADS)

    Westbrooke, Eboni F.

    Nickel-base superalloys, with gamma/gamma' microstructure, are the primary material used in turbines for aerospace applications. The blades in the hottest region of the turbine engine are made of single crystal Ni-base superalloys. It has been shown that the critical resolved shear stress (CRSS) of these materials is orientation dependent (also known as non-Schmid effect). The purpose of this research was to investigate the plastic deformation mechanisms of single crystal Ni-base superalloys as a function of crystallographic orientation in order to understand the factors that contribute to the non-Schmid effect. The superalloys in this study possessed alloying elements in amounts which defined them as 1st and 2nd generation superalloys. Tensile samples of various orientations were loaded to different strain levels. The mechanisms of plastic deformation were characterized by optical and scanning electron microscopy (SEM) observations of deformation bands as well as the dislocation structures using transmission electron microscopy (TEM). It was confirmed that the CRSS of the single crystals did not follow Schmid's law and the near <111> specimens showed the lowest values. The degree of non-Schmid behavior in the <111> specimens was diminished by HIP'ing, which resulted in closure of solidification pores. Furthermore, it was shown that the CRSS for the <100> loaded samples was smallest when loaded along the secondary dendrite arms. The slip analysis by optical microscopy showed that the deformation bands did not follow the expected {111} slip planes for all samples. Studies in SEM proved that those slip bands that followed the {111} planes were associated with extensive shearing of gamma' particles. In addition, it was found that the presence of tri-axial stress states within the macrostructure influenced the deformation path significantly. The TEM observations of deformed specimens revealed that plastic deformation took place mainly in the gamma channels in specimens

  14. 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.

  15. A continuum model for the creep of single crystal nickel-base superalloys

    SciTech Connect

    Prasad, Sharat C.; Rao, I.J.; Rajagopal, K.R. . E-mail: krajagopal@mengr.tamu.edu

    2005-02-01

    In this paper, we develop a constitutive theory within a thermodynamic setting to describe the creep of single crystal superalloys that gainfully exploits the fact that the configuration that the body would attain on the removal of the external stimuli, referred to as the 'natural configuration', evolves, with the response of the body being elastic from these evolving natural configurations. The evolution of the natural configurations is determined by the tendency of the body to undergo a process that maximizes the rate of dissipation. Here, the elastic response is assumed to be linearly elastic with cubic symmetry associated with the body which remains the same as the configuration evolves. A form for the inelastic stored energy (the energy that is 'trapped' within dislocation networks) is utilized based on simple ideas related to the motion of the dislocations. The rate of dissipation is assumed to be proportional to the density of mobile dislocations and another term that takes into account the damage accumulation due to creep. The model developed herein is used to simulate uniaxial creep of <0 0 1> oriented single crystal nickel-base superalloys. The predictions of the theory agree well with the available experimental data for CMSX-4.

  16. 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

  17. Elevated temperature creep-rupture behavior of the single crystal nickel-base superalloy NASAIR 100

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Ebert, L. J.

    1985-01-01

    The creep and rupture behavior of 001-line-oriented single crystals of the nickel-base superalloy NASAIR 100 was investigated at temperatures of 925 and 1000 C. In the stress and temperature ranges studied, the steady state creep rate, time to failure, time to the onset of secondary creep, and the time to the onset of tertiary creep all exhibited power law dependencies on the applied stress. The creep rate exponents for this alloy were between seven and eight, and the modulus-corrected activation energy for creep was approximately 350 kjoule/mole, which was comparable to the measured activation energy for Ostwald ripening of the gamma-prime precipitates. Oriented gamma-prime coarsening to form lamellae perpendicular to the applied stress was very prominent during creep. At 1000 C, the formation of a continuous gamma-gamma-prime lamellar structure was completed during the primary creep stage. Shear through the gamma-gamma-prime interface is considerd to be the rate limiting step in the deformation process. Gradual thickening of the lamellae appeared to be the cause of the onset of tertiary creep. At 925 C, the fully developed lamellar structure was not achieved until the secondary or tertiary creep stages. At this temperature, the gamma-gamma-prime lamellar structure did not appear to be as beneficial for creep resistance as at the higher temperature.

  18. Anisotropic constitutive model for nickel base single crystal alloys: Development and finite element implementation

    NASA Technical Reports Server (NTRS)

    Dame, L. T.; Stouffer, D. C.

    1986-01-01

    A tool for the mechanical analysis of nickel base single crystal superalloys, specifically Rene N4, used in gas turbine engine components is developed. This is achieved by a rate dependent anisotropic constitutive model implemented in a nonlinear three dimensional finite element code. The constitutive model is developed from metallurigical concepts utilizing a crystallographic approach. A non Schmid's law formulation is used to model the tension/compression asymmetry and orientation dependence in octahedral slip. Schmid's law is a good approximation to the inelastic response of the material in cube slip. The constitutive equations model the tensile behavior, creep response, and strain rate sensitivity of these alloys. Methods for deriving the material constants from standard tests are presented. The finite element implementation utilizes an initial strain method and twenty noded isoparametric solid elements. The ability to model piecewise linear load histories is included in the finite element code. The constitutive equations are accurately and economically integrated using a second order Adams-Moulton predictor-corrector method with a dynamic time incrementing procedure. Computed results from the finite element code are compared with experimental data for tensile, creep and cyclic tests at 760 deg C. The strain rate sensitivity and stress relaxation capabilities of the model are evaluated.

  19. 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.

  20. Optimization of Weld Conditions and Alloy Composition for Welding of Single-Crystal Nickel-Based Superalloys

    SciTech Connect

    Vitek, John Michael; David, Stan A; Babu, Sudarsanam S

    2007-01-01

    Calculations were carried out to identify optimum welding conditions and weld alloy compositions to avoid stray grain formation during welding of single-crystal nickel-based superalloys. The calculations were performed using a combination of three models: a thermal model to describe the weld pool shape and the local thermal gradient and solidification front velocity; a geometric model to identify the local active dendrite growth variant, and a nucleation and growth model to describe the extent of stray grain formation ahead of the advancing solidification front. Optimum welding conditions (low weld power, high weld speed) were identified from the model calculations. Additional calculations were made to determine potential alloy modifications that reduce the solidification temperature range while maintaining high gamma prime content. The combination of optimum weld conditions and alloy compositions should allow for weld repair of single-crystal nickel-based superalloys without sacrificing properties or performance.

  1. Influence of composition on microstructural parameters of single crystal nickel-base superalloys

    SciTech Connect

    MacKay, R.A.; Gabb, T.P.; Garg, A.; Rogers, R.B.; Nathal, M.V.

    2012-08-15

    Fourteen nickel-base superalloy single crystals containing a range of chromium (Cr), cobalt (Co), molybdenum (Mo), and rhenium (Re) levels, and fixed amounts of aluminum (Al) and tantalum (Ta), were examined to determine the effect of bulk composition on basic microstructural parameters, including {gamma} Prime solvus, {gamma} Prime volume fraction, topologically close-packed (TCP) phases, {gamma} and {gamma} Prime phase chemistries, and {gamma}-{gamma} Prime lattice mismatch. Regression models describing the influence of bulk alloy composition on each of the microstructural parameters were developed and compared to predictions by a commercially-available software tool that used computational thermodynamics. Co produced the largest change in {gamma} Prime solvus over the wide compositional range explored and Mo produced the biggest effect on the {gamma} lattice parameter over its range, although Re had a very potent influence on all microstructural parameters investigated. Changing the Cr, Co, Mo, and Re contents in the bulk alloy had an impact on their concentrations in the {gamma} matrix and to a smaller extent in the {gamma} Prime phase. The software tool under-predicted {gamma} Prime solvus temperatures and {gamma} Prime volume fractions, and over-predicted TCP phase volume fractions at 982 Degree-Sign C. However, the statistical regression models provided excellent estimations of the microstructural parameters and demonstrated the usefulness of such formulas. - Highlights: Black-Right-Pointing-Pointer Effects of Cr, Co, Mo, and Re on microstructure in new low density superalloys Black-Right-Pointing-Pointer Co produced a large change in {gamma} Prime solvus; Mo had a large effect on lattice mismatch. Black-Right-Pointing-Pointer Re exhibited very potent influence on all microstructural parameters was investigated. Black-Right-Pointing-Pointer {gamma} and {gamma} Prime phase chemistries both varied with temperature and alloy composition. Black

  2. The impact of carbon on single crystal nickel-base superalloys: Carbide behavior and alloy performance

    NASA Astrophysics Data System (ADS)

    Wasson, Andrew Jay

    Advanced single crystal nickel-base superalloys are prone to the formation of casting grain defects, which hinders their practical implementation in large gas turbine components. Additions of carbon (C) have recently been identified as a means of reducing grain defects, but the full impact of C on single crystal superalloy behavior is not entirely understood. A study was conducted to determine the effects of C and other minor elemental additions on the behavior of CMSX-4, a commercially relevant 2nd generation single crystal superalloy. Baseline CMSX-4 and three alloy modifications (CMSX-4 + 0.05 wt. % C, CMSX-4 + 0.05 wt. % C and 68 ppm boron (B), and CMSX-4 + 0.05 wt. % C and 23 ppm nitrogen (N)) were heat treated before being tested in high temperature creep and high cycle fatigue (HCF). Select samples were subjected to long term thermal exposure (1000 °C/1000 hrs) to assess microstructural stability. The C modifications resulted in significant differences in microstructure and alloy performance as compared to the baseline. These variations were generally attributed to the behavior of carbide phases in the alloy modifications. The C modification and the C+B modification, which both exhibited script carbide networks, were 25% more effective than the C+N modification (small blocky carbides) and 10% more effective than the baseline at preventing grain defects in cast bars. All C-modified alloys exhibited reduced as-cast gamma/gamma' eutectic and increased casting porosity as compared to baseline CMSX-4. The higher levels of porosity (volume fractions 0.002 - 0.005 greater than the baseline) were attributed to carbides blocking molten fluid flow during the final stages of solidification. Although the minor additions resulted in reduced solidus temperature by up to 16 °C, all alloys were successfully heat treated without incipient melting by modifying commercial heat treatment schedules. In the B-containing alloy, heat treatment resulted in the transformation of

  3. Microstructure Evolution and Analysis of A [011] Orientation, Single-Crystal, Nickel-Based Superalloy During Tensile Creep

    NASA Astrophysics Data System (ADS)

    Tian, Sugui; Zhang, Shu; Li, Chenxi; Yu, Huichen; Su, Yong; Yu, Xingfu; Yu, Lili

    2012-10-01

    By means of the elastic-plastic finite-element method (FEM) for calculating the distribution features of the von Mises stress and strain energy density, the influences of the applied stress on the von Mises stress of the γ'/ γ phases and the rafting of the γ' phase for the [011] orientation, single-crystal, nickel-based superalloy are investigated. The results show that, after being fully heat treated, the microstructure of the [011] orientation, single-crystal, nickel-based superalloy consists of the cuboidal γ' phase embedded coherently in the γ matrix, and the cuboidal γ' phase on (100) plane is regularly arranged along a 45 deg angle relative to the [011] orientation. Compared with the matrix channel of [010] orientation, the bigger von Mises stress is produced within the [001] matrix channel when the tensile stress is applied along the [011] orientation. Under the action of the larger principal stress component, the bigger expanding lattice strain occurs on the (001) plane of the cuboidal γ' phase along the [010] direction, which may trap the Al, Ti atoms with a bigger atomic radius for promoting the directional growth of the γ' phase into the stripe-like rafted structure along the [001] orientation. The changes of the interatomic potential energy, misfit stress, and interfacial energy during the tensile creep are thought to be the driving forces of promoting the elements' diffusion and directional growth of the γ' phase.

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

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.

    1981-01-01

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

  5. Modeling of abnormal mechanical properties of nickel-based single crystal superalloy by three-dimensional discrete dislocation dynamics

    NASA Astrophysics Data System (ADS)

    Yang, Hui; Li, Zhenhuan; Huang, Minsheng

    2014-12-01

    Unlike common single crystals, the nickel-based single crystal superalloy shows surprisingly anomalous flow strength (i.e. with the increase of temperature, the yield strength first increases to a peak value and then decreases) and tension-compression (TC) asymmetry. A comprehensive three-dimensional discrete dislocation dynamics (3D-DDD) procedure was developed to model these abnormal mechanical properties. For this purpose, a series of complicated dynamic evolution details of Kear-Wilsdorf (KW) locks, which are closely related to the flow strength anomaly and TC asymmetry, were incorporated into this 3D-DDD framework. Moreover, the activation of the cubic slip system, which is the origin of the decrease in yield strength with increasing temperature at relatively high temperatures, was especially taken into account by introducing a competition criterion between the unlocking of the KW locks and the activation of the cubic slip system. To test our framework, a series of 3D-DDD simulations were performed on a representative volume cell model with a cuboidal Ni3Al precipitate phase embedded in a nickel matrix. Results show that the present 3D-DDD procedure can successfully capture the dynamic evolution of KW locks, the flow strength anomaly and TC asymmetry. Then, the underlying dislocation mechanisms leading to these abnormal mechanical responses were investigated and discussed in detail. Finally, a cyclic deformation of the nickel-based single crystal superalloy was modeled by using the present DDD model, with a special focus on the influence of KW locks on the Bauschinger effect and cyclic softening.

  6. LCF behavior and life prediction method of a single crystal nickel-based superalloy at high temperature

    NASA Astrophysics Data System (ADS)

    Zhang, Zhihua; Yu, Huichen; Dong, Chengli

    2015-12-01

    Low cycle fatigue tests were conducted on the single crystal nickel-based superalloy, DD6, with different crystallographic orientations (i.e., [001], [011], and [111]) and strain dwell types (i.e., tensile, compressive, and balanced types) at a certain high temperature. Given the material anisotropy and mean stress, both orientation factor and stress range were introduced to the Smith,Watson, and Topper (SWT) stress model to predict the fatigue life. Experimental results indicated that the fatigue properties of DD6 depend on both crystallographic orientation and loading types. The fatigue life of the tensile, compressive, and balanced strain dwell tests are shorter than those of continuous cycling tests without strain dwell because of the important creep effect. The predicted results of the proposed modified SWT stress method agree well with the experimental data.

  7. Twinning Behaviors During Thermomechanical Fatigue Cycling of a Nickel-Base Single-Crystal TMS-82 Superalloy

    NASA Astrophysics Data System (ADS)

    Lv, X. Z.; Zhang, J. X.; Harada, H.

    2014-03-01

    This paper provides further insight into the formation of deformation twins at different stages during the whole thermomechanical fatigue cycling in a nickel-base single-crystal TMS-82 superalloy. In general, it is found that twinning behaviors can always be associated with the applied stress orientation. The preferred twinning direction at the primary stage is <001>-compression since the tangled dislocations which appear after the first plastic deformation provide an opportunity for twinning nucleation in compression. At the intermediate stage, the applied stress required for formation of twins in tension is much larger than that in compression; hence, twinning behaviors show distinct tension/compression asymmetry. A thick twin plate and a great many dislocations can be found after fatigue failure, and one can rationalize the reason for this twinning being associated with the TMF procedure. Twins at the tip of the crack in tension occur owing to the existence of compressive strain field.

  8. High temperature low-cycle fatigue mechanisms in single crystals of nickel-based superalloy Mar-M 200

    NASA Technical Reports Server (NTRS)

    Milligan, W. W.; Jayaraman, N.

    1984-01-01

    Twenty three high temperature low-cycle fatigue tests were conducted on single crystals of the nickel-based superalloy Mar-M 200. Tests were conducted at 760 and 870 C. SEM fractography and transmission electron microscopy were used to determine mechanisms responsible for the observed orientation dependent fatigue behavior. It has been concluded that the plastic characteristics of the alloy lead to orientation-dependent strain hardening and fatigue lives at 760 C. At 870 C, the elastic characteristics of the alloy dominated the behavior, even though the plastic strain ranges were about the same as they were at 760 C. This led to orientation-dependent fatigue lives, but the trends were not the same as they were at 760 C.

  9. The influence of cobalt, tantalum, and tungsten on the elevated temperature mechanical properties of single crystal nickel-base superalloys

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Ebert, L. J.

    1985-01-01

    The influence of composition on the tensile and creep strength of 001-line oriented nickel-base superalloy single crystals at temperatures near 1000 C was investigated. Cobalt, tantalum, and tungsten concentrations were varied according to a matrix of compositions based on the single crystal version of MAR-M247. For alloys with the baseline refractory metal level of 3 wt pct Ta and 10 wt pct W, decreases in Co level from 10 to 0 wt pct resulted in increased tensile and creep strength. Substitution of 2 wt pct W for 3 wt pct Ta resulted in decreased creep life at high stresses, but improved life at low stresses. Substitution of Ni for Ta caused large reductions in tensile strength and creep resistance, and corresponding increases in ductility. For these alloys with low Ta-plus-W totals, strength was independent of Co level. The effects of composition on properties were related to the microstructural features of the alloys. In general, high creep strength was associated with high levels of gamma-prime volume fraction, gamma-gamma-prime lattice mismatch, and solid solution hardening.

  10. Influence of molybdenum on the creep properties of nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.; Nathal, M. V.; Pearson, D. D.

    1990-01-01

    The Mo content of an alloy series based on Ni-6 wt pct Al-6 wt pct Ta was systematically varied from 9.8 to 14.6 wt pct, in order to ascertain the influence of Mo on the creep properties of single crystals. The optimum initial gamma-gamma prime microstructure for raft development and creep strength was established in each alloy before testing. It was found that, as the Mo content increased from 9.8 to 14.0 percent, the magnitude of the lattice mismatch increased; upon reaching 14.6 percent, a degradation of mechanical properties occurred due to the precipitation of a third phase. These results suggest that small refractory metal content and initial gamma-prime variations can profoundly affect mechanical properties.

  11. Micromechanisms of fatigue crack growth in a single crystal Inconel 718 nickel-based superalloy

    SciTech Connect

    Mercer, C.; Soboyejo, A.B.O.; Soboyejo, W.O. )

    1999-07-09

    The fatigue crack growth behavior of an experimental, single crystal alloy, of equivalent nominal chemical composition to Inconel 718 is presented. Fracture modes under cyclic loading were determined by scanning electron microscopy. The results of the fractographic analyses are presented on a fracture mechanism map that shows the dependence of the fatigue fracture mechanisms on the maximum stress intensity factor, K[sub max], and the stress intensity factor range, [Delta]K. Crack-tip deformation mechanisms associated with fatigue crack growth were studied using transmission electron microscopy. The relative effects of [Delta]K and K[sub max] on the fatigue crack growth behavior of this material are discussed within the context of a two-parameter crack growth law. The influence of grain boundaries on the fatigue crack growth resistance of materials such as Inconel 718 is also discussed in light of the results of this investigation.

  12. Effects of Microstructural Parameters on Creep of Nickel-Base Superalloy Single Crystals

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

    Microstructure-sensitive creep models have been developed for Ni-base superalloy single crystals. Creep rupture testing was conducted on fourteen single crystal alloys at two applied stress levels at each of two temperatures, 982 and 1093 C. The variation in creep lives among the different alloys could be explained with regression models containing relatively few microstructural parameters. At 982 C, gamma-gamma prime lattice mismatch, gamma prime volume fraction, and initial gamma prime size were statistically significant in explaining the creep rupture lives. At 1093 C, only lattice mismatch and gamma prime volume fraction were significant. These models could explain from 84 to 94 percent of the variation in creep lives, depending on test condition. Longer creep lives were associated with alloys having more negative lattice mismatch, lower gamma prime volume fractions, and finer gamma prime sizes. The gamma-gamma prime lattice mismatch exhibited the strongest influence of all the microstructural parameters at both temperatures. Although a majority of the alloys in this study were stable with respect to topologically close packed (TCP) phases, it appeared that up to approximately 2 vol% TCP phase did not affect the 1093 C creep lives under applied stresses that produced lives of approximately 200 to 300 h. In contrast, TCP phase contents of approximately 2 vol% were detrimental at lower applied stresses where creep lives were longer. A regression model was also developed for the as-heat treated initial gamma prime size; this model showed that gamma prime solvus temperature, gamma-gamma prime lattice mismatch, and bulk Re content were all statistically significant.

  13. Creep property and microstructure evolution of a nickel-base single crystal superalloy in [011] orientation

    SciTech Connect

    Han, G.M. Yu, J.J.; Hu, Z.Q.; Sun, X.F.

    2013-12-15

    The creep property and microstructure evolution of a single crystal superalloy with [011] orientation were investigated at the temperatures of 700 °C, 900 °C and 1040 °C. It is shown that there exist stages of primary, steady-state, and tertiary creep under the lower temperature 700 °C. As the temperature increases to high temperatures of 900 °C and 1040 °C, steady-state creep stage is reduced or disappears and the shape of creep curves is dominated by an extensive tertiary stage. The minimum creep strain rate exhibits power law dependence on the applied stress; the stress exponents at 700 °C, 900 °C and 1040 °C are 28, 13 and 6.5, respectively. Microstructure observation shows that the morphologies of γ′ phase almost keep original shape at the lower temperature 700 °C and high applied stress. With the increasing creep temperature, γ′ precipitates tend to link together and form lamellar structure at an angle of 45° inclined to the applied stress. Transmission electron microscopy (TEM) investigations reveal that multiple < 110 > (111) slip systems gliding in the matrix channels and shearing γ′ precipitates by stacking faults or bending dislocation pairs are the main deformation mechanism at the lower temperature of 700 °C. At the high temperatures of 900 °C and 1040 °C, dislocation networks are formed at γ/γ′ interfaces and the γ′ rafts are sheared by dislocation pairs. - Highlights: • Creep properties of < 011 >-oriented single crystal superalloys were investigated. • γ′ phases become rafting at an angle of 45° inclined to the applied stress. • Creep deformation mechanisms depend on temperature and stress.

  14. Growth Stresses in Thermally Grown Oxides on Nickel-Based Single-Crystal Alloys

    NASA Astrophysics Data System (ADS)

    Rettberg, Luke H.; Laux, Britta; He, Ming Y.; Hovis, David; Heuer, Arthur H.; Pollock, Tresa M.

    2016-03-01

    Growth stresses that develop in α-Al2O3 scale that form during isothermal oxidation of three Ni-based single crystal alloys have been studied to elucidate their role in coating and substrate degradation at elevated temperatures. Piezospectroscopy measurements at room temperature indicate large room temperature compressive stresses in the oxides formed at 1255 K or 1366 K (982 °C or 1093 °C) on the alloys, ranging from a high of 4.8 GPa for René N4 at 1366 K (1093 °C) to a low of 3.8 GPa for René N5 at 1255 K (982 °C). Finite element modeling of each of these systems to account for differences in coefficients of thermal expansion of the oxide and substrate indicates growth strains in the range from 0.21 to 0.44 pct at the oxidation temperature, which is an order of magnitude higher than the growth strains measured in the oxides on intermetallic coatings that are typically applied to these superalloys. The magnitudes of the growth strains do not scale with the parabolic oxidation rate constants measured for the alloys. Significant spatial inhomogeneities in the growth stresses were observed, due to (i) the presence of dendritic segregation and (ii) large carbides in the material that locally disrupts the structure of the oxide scale. The implications of these observations for failure during cyclic oxidation, fatigue cycling, and alloy design are considered.

  15. Effect of hydrogen on deformation structure and properties of CMSX-2 nickel-base single-crystal superalloy

    NASA Technical Reports Server (NTRS)

    Dollar, M.; Bernstein, I. M.; Walston, S.; Prinz, F.; Domnanovich, A.

    1987-01-01

    Material used in this study was a heat of the alloy CMSX-2. This nickel-based superalloy was provided in the form of oriented single crystals, solutionized for 3 hrs at 1315 C. It was then usually heat treated as follows: 1050 C/16h/air cool + 850 C/48h/air cool. The resulting microstructure is dominated by cuboidal, ordered gamma precipitates with a volume fraction of about 75% and an average size of 0.5 microns. In brief, the most compelling hydrogen induced-changes in deformation structure are: (1) enhanced dislocation accumulation in the gamma matrix; and (2) more extensive cross-slip of superdislocations in the gamma precipitates. The enhanced dislocation density in gamma acts to decrease the mean free path of a superdislocation, while easier cross slip hinders superdislocation movement by providing pinning points in the form of sessile jobs. Both processes contribute to the increase of flow stress and the notable work hardening that occurs prior to fracture.

  16. The influence of cobalt, tantalum, and tungsten on the microstructure of single crystal nickel-base superalloys

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Ebert, L. J.

    1985-01-01

    The influence of composition on the microstructure of single crystal nickel-base superalloys was investigated. Co was replaced by Ni, and Ta was replaced by either Ni or W, according to a matrix of compositions based on MAR-M247. Substitution of Ni for Co caused an increase in gamma-prime solvus temperature, an increase in gamma-gamma-prime lattice mismatch, and the precipitation of W-rich phases in the alloys with high refractory metal levels. Substitution of Ni for Ta caused large decreases in gamma-prime solvus temperature, gamma-prime volume fraction, and gamma-gamma-prime lattice mismatch, whereas substitution of W for Ta resulted in smaller decreases in these features. For the alloys with gamma-prime particles that remained coherent, substitution of Ni for Co caused an increase in gamma-prime coarsening rate. The two alloys with the largest magnitude of lattice mismatch possessed gamma-prime particles which lost coherency during unstressed aging and exhibited anomalously low coarsening rates. Creep exposure at 1000 C resulted in the formation of gamma-prime lamellae oriented perpendicular to the applied stress axis in all alloys.

  17. Microstructure evolution and FEM analysis of a [111] oriented single crystal nickel-based superalloy during tensile creep

    NASA Astrophysics Data System (ADS)

    Tian, Sugui; Li, Qiuyang; Su, Yong; Yu, Huichen; Xie, Jun; Zhang, Shu

    2015-03-01

    By means of the elastic-plastic stress-strain finite element method (FEM), the distribution of the von Mises stress and strain energy density in the regions near the interfaces of the cuboidal γ/ γ' phases is calculated to investigate the rafted behaviors of γ' phase in a [111] oriented single crystal (SC) nickel-based superalloy. Results show that, after fully heat treated, the microstructure of the superalloy consists of the cuboidal γ' phase embedded coherently in the γ matrix and arranged regularly along the <100> orientation. And the parameters and misfits of γ'/ γ phases in the alloy increase with the temperature. After crept for 50 h, the γ' phase in alloy has transformed into the mesh-like rafted structure on (010) plane along [001] and [100] orientations. When the tensile stress is applied along [111] direction, the change of the strain energy on the planes of the cuboidal γ' phase results in the directional diffusion of the elements. Thereinto, compared with (010) plane, the bigger expanding strain occurs on (100) and (001) planes along the [010], [001] and [010], [100] directions, which may trap the Al and Ti atoms with bigger radius to promote the directional growth of γ' phase on (010) plane along [100] and [001] directions. This is thought to be the main reason for the γ' phase directionally growing into the mesh-like rafted structure on (010) plane.

  18. The Cyclic Stress-Strain Behavior of a Single Crystal Nickel-Base Superalloy. Ph.D. Thesis

    NASA Technical Reports Server (NTRS)

    Gabb, Timothy P.

    1988-01-01

    The cyclic stress-strain response and similar deformation structures of the single crystal nickel based superalloy was described under a specific set of conditions. The isothermal low cycle fatigue response and deformation structures were described at a typical intermediate temperature and at high temperature. Specimens oriented near the (001) and (111) crystallographic orientations were tested at 1050 C, where more moderate orientation effects were expected. This enabled the description of the deformation structures at each of the 2 temperatures and their relationship to the observed cyclic stress-strain behavior. The initial yield strength of all specimens tested at 650 C was controlled by the shearing of the gamma prime precipitates by dislocation pairs. Low cycle fatigue tests at 650 C had cyclic hardening, which was associated with dislocation interactions in the gamma matrix. The initial yield strength of specimens tested at 1050 C was associated with dislocation bypassing of the gamma prime precipitates. Low cycle fatigue tests at 1050 C had cyclic softening, associated with extensive dislocation recovery at the gamma-gamma prime interfaces along with some gamma prime precipitate coarsening.

  19. Local x-ray diffraction analysis of the structure of dendrites in single-crystal nickel-base superalloys

    SciTech Connect

    Brueckner, U.; Epishin, A.; Link, T.

    1997-12-01

    The structure of the dendrites in the single-crystal nickel-base superalloys SC16, SRR99 and CMSX4 with different refractory element levels (Mo + Ta + W + Re) has been investigated by local X-ray diffraction. A special technique was used to improve the spatial resolution of the X-ray diffraction and to enable the precise control of the X-ray spot position within the dendritic structure. A significant change of the {gamma}/{gamma}{prime}-lattice misfit was found within the dendrite in the superalloys with higher refractory element levels SRR99 and CMSX4. The observed misfit change is based on the change of the {gamma}-lattice parameter due to segregation of W and Re. The intensity of the X-ray beam reflected from the dendrite periphery was found to be weaker than that from the dendrite centre because of the mosaicity. Therefore misfit measurements without knowledge of the X-ray spot position in the dendritic structure lead to values that correspond more to the dendrite core.

  20. Ta effect on oxidation of a nickel-based single-crystal superalloy and its sputtered nanocrystalline coating at 900-1100 °C

    NASA Astrophysics Data System (ADS)

    Wang, Jinlong; Chen, Minghui; Zhu, Shenglong; Wang, Fuhui

    2015-08-01

    Sputtering nanocrystalline coating was prepared on a nickel-based single-crystal superalloy N5. The oxidation behavior of the superalloy substrate and its nanocrystalline coating was investigated at 900-1100 °C. Results indicated that the nanocrystalline coating enhanced the oxidation and scale spallation resistance of the single-crystal superalloy. Elements interdiffusion has not occurred between the substrate and coating. Refractory element, Ta, inherently contained in N5, had a significant effect on the scale microstructure and oxidation behavior of both the single-crystal superalloy substrate and its sputtering nanocrystalline coating.

  1. Analyses of Elemental Partitioning in Advanced Nickel-Base Superalloy Single Crystals

    NASA Technical Reports Server (NTRS)

    Dreshfield, Robert L.; Thomas, Kimberly J.

    2005-01-01

    Aircraft propulsion engines for the High Speed Civil Transport which may be developed early in the 21st century will require significantly different durability requirements than those which currently power civil aircraft. The durability will be more difficult to achieve because it is expected that the new aircraft engines will have to operate at near maximum power for more than half of each flight compared to 5 to 10 percent for typical current aircraft. To meet this requirement, a team of NASA, Pratt & Whitney Aircraft, and General Electric personnel have been formed to develop an appropriate alloy for the mission. This report summarizes the work performed by a part of that team up to the retirement of one of its members, R.L. Dreshfield. The prime purpose of the report is to assemble the data obtained in a single document so that it may be more accessible to those who may wish to pursue it at a later date.

  2. Effect of minor carbon additions on the high-temperature creep behavior of a single-crystal nickel-based superalloy

    SciTech Connect

    Wang, L. Wang, D.; Liu, T.; Li, X.W.; Jiang, W.G.; Zhang, G.; Lou, L.H.

    2015-06-15

    Different amounts of carbon were added to a single-crystal nickel-based superalloy. The microstructural evolution of these alloys before and after high-temperature creep tests was investigated by employing scanning electron microscopy and transmission electron microscopy. Upon increasing the carbon contents, the volume fraction and diameter of the carbides increased gradually: however, the creep lives of the alloys increased slightly at first and subsequently decreased. The formation of second-phase particles, such as the nano-sized M{sub 23}C{sub 6}, blocky and needle-shaped μ phase, was observed in the creep samples, which was closely related to the high-temperature creep behaviors. - Highlights: • Creep behaviors of alloys with different amounts of carbon were investigated. • The creep rupture lives increased and later decreased with more carbon. • Second-phase particles were responsible for the different creep behaviors.

  3. Quantitative experimental determination of the solid solution hardening potential of rhenium, tungsten and molybdenum in single-crystal nickel-based superalloys

    DOE PAGESBeta

    Fleischmann, Ernst; Miller, Michael K.; Affeldt, Ernst; Glatzel, Uwe

    2015-01-31

    Here, the solid-solution hardening potential of the refractory elements rhenium, tungsten and molybdenum in the matrix of single-crystal nickel-based superalloys was experimentally quantified. Single-phase alloys with the composition of the nickel solid-solution matrix of superalloys were cast as single crystals, and tested in creep at 980 °C and 30–75 MPa. The use of single-phase single-crystalline material ensures very clean data because no grain boundary or particle strengthening effects interfere with the solid-solution hardening. This makes it possible to quantify the amount of rhenium, tungsten and molybdenum necessary to reduce the creep rate by a factor of 10. Rhenium is moremore » than two times more effective for matrix strengthening than either tungsten or molybdenum. The existence of rhenium clusters as a possible reason for the strong strengthening effect is excluded as a result of atom probe tomography measurements. If the partitioning coefficient of rhenium, tungsten and molybdenum between the γ matrix and the γ' precipitates is taken into account, the effectiveness of the alloying elements in two-phase superalloys can be calculated and the rhenium effect can be explained.« less

  4. Quantitative experimental determination of the solid solution hardening potential of rhenium, tungsten and molybdenum in single-crystal nickel-based superalloys

    SciTech Connect

    Fleischmann, Ernst; Miller, Michael K.; Affeldt, Ernst; Glatzel, Uwe

    2015-01-31

    Here, the solid-solution hardening potential of the refractory elements rhenium, tungsten and molybdenum in the matrix of single-crystal nickel-based superalloys was experimentally quantified. Single-phase alloys with the composition of the nickel solid-solution matrix of superalloys were cast as single crystals, and tested in creep at 980 °C and 30–75 MPa. The use of single-phase single-crystalline material ensures very clean data because no grain boundary or particle strengthening effects interfere with the solid-solution hardening. This makes it possible to quantify the amount of rhenium, tungsten and molybdenum necessary to reduce the creep rate by a factor of 10. Rhenium is more than two times more effective for matrix strengthening than either tungsten or molybdenum. The existence of rhenium clusters as a possible reason for the strong strengthening effect is excluded as a result of atom probe tomography measurements. If the partitioning coefficient of rhenium, tungsten and molybdenum between the γ matrix and the γ' precipitates is taken into account, the effectiveness of the alloying elements in two-phase superalloys can be calculated and the rhenium effect can be explained.

  5. Effect of Surface Preparation on the 815°C Oxidation of Single-Crystal Nickel-Based Superalloys

    NASA Astrophysics Data System (ADS)

    Sudbrack, Chantal K.; Beckett, Devon L.; MacKay, Rebecca A.

    2015-11-01

    A primary application for single-crystal superalloys has been jet engine turbine blades, where operation temperatures reach well above 1000°C. The NASA Glenn Research Center is considering use of single-crystal alloys for future, lower temperature application in the rims of jet engine turbine disks. Mechanical and environmental properties required for potential disk rim operation at 815°C are being examined, including the oxidation and corrosion behavior, where there is little documentation at intermediate temperatures. In this study, single-crystal superalloys, LDS-1101+Hf and CMSX-4+Y, were prepared with different surface finishes and compared after isothermal and cyclic oxidation exposures. Surface finish has a clear effect on oxide formation at 815°C. Machined low-stress ground surfaces after exposure for 440 h produce thin Al2O3 external scales, which is consistent with higher temperature oxidation, whereas polished surfaces with a mirror finish yield much thicker NiO external scales with subscale of Cr2O3-spinel-Al2O3, which may offer less reliable oxidation resistance. Additional experiments separate the roles of cold-work, localized deformation, and the extent of polishing and surface roughness on oxide formation.

  6. Factors which influence directional coarsening of gamma-prime during creep in nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.; Ebert, L. J.

    1984-01-01

    Changes in the morphology of the gamma prime precipitate were examined as a function of the time during creep at 982 C in 001 oriented single crystals of a Ni-Al-Mo-Ta superalloy. In this alloy, which has a large negative misfit of -0.80 pct., the gamma prime particles link together during creep to form platelets, or rafts, which are aligned with their broad faces perpendicular to the applied tensile axis. The effects of initial microstructure and alloy composition of raft development and creep properties were investigated. Directional coarsening of gamma prime begins during primary creep and continues well after the onset of second state creep. The thickness of the rafts remains constant up through the onset of tertiary creep, a clear indication of the stability of the finely-spaced gamma/gamma prime lamellar structure. The thickness of the rafts which formed was equal to the initial gamma prime size which was present prior to testing. The single crystals with the finest gamma prime size exhibited the longest creep lives, because the resultant rafted structure had a larger number of gamma/gamma prime interfaces per unit volume of material. Reducing the Mo content by only 0.73 wt. pct. increased the creep life by a factor of three, because the precipitation of a third phase was eliminated.

  7. Factors which influence directional coarsening of Gamma prime during creep in nickel-base superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.; Ebert, L. J.

    1984-01-01

    Changes in the morphology of the gamma prime precipitate were examined as a function of time during creep at 982 C in 001 oriented single crystals of a Ni-Al-Mo-Ta superalloy. In this alloy, which has a large negative misfit of -0.80 pct., the gamma prime particles link together during creep to form platelets, or rafts, which are aligned with their broad faces perpendicular to the applied tensile axis. The effects of initial microstructure and alloy composition of raft development and creep properties were investigated. Directional coarsening of gamma prime begins during primary creep and continues well after the onset of second state creep. The thickness of the rafts remains constant up through the onset of tertiary creep a clear indication of the stability of the finely-spaced gamma/gamma prime lamellar structure. The thickness of the rafts which formed was equal to the initial gamma prime size which was present prior to testing. The single crystals with the finest gamma prime size exhibited the longest creep lives, because the resultant rafted structure had a larger number of gamma/gamma prime interfaces per unit volume of material. Reducing the Mo content by only 0.73 wt. pct. increased the creep life by a factor of three, because the precipitation of a third phase was eliminated.

  8. The role of the gamma/gamma-prime eutectic and porosity on the tensile behavior of a single-crystal nickel-base superalloy

    NASA Technical Reports Server (NTRS)

    Walston, W. S.; Bernstein, I. M.; Thompson, A. W.

    1991-01-01

    The microstructure of a single-crystal nickel-base superalloy, PWA 1480, has been varied by heat treatment and hot isostatic pressing in order to study the role of the gamma/gamma-prime eutectic and porosity on subsequent tensile behavior. The level of porosity was found not to affect any of the tensile properties, while the gamma/gamma-prime eutectic strongly influenced ductility. Eliminating the gamma/gamma-prime eutectic increased ductility which was attributed to the cleavage fracture of this constituent. It is proposed that such cleavage of the gamma/gamma-prime eutectic is initiated by the stress created from impinging slip bands, promoting shear localization, and final fracture along 111 slip planes. The precise nature of this fracture process is discussed, with emphasis on the role of the gamma/gamma-prime microstructure. The deformation structure of PWA 1480 was also studied, and while different in some respects from many other single-crystal superalloys, its fracture process appears to be similar.

  9. The Growth of Naturally-Generated Small Fatigue Cracks in a Nickel-Base Single-Crystal Superalloy

    NASA Astrophysics Data System (ADS)

    Yandt, Scott A.

    An experimental and analytical study on the formation and growth small fatigue cracks embedded in a notch in single-crystal superalloy has been investigated. The experimental program consisted of 12 constant amplitude fatigue tests performed on single-edge notch (SEN) fatigue specimens oriented with the loading axis along [010] and with a notch factor of 2.7. The fatigue tests concentrated on one temperature (650°C) and loading condition with the secondary crystallographic orientation---the notch orientation---being the primary variable. Two secondary crystallographic orientations were considered in the present study, [101] and [100]. In the analytical study, the distribution of stresses and strains in the notch region and the stress-intensity factors and the elastic-plastic J-integral for Mode-I semi-elliptical surface cracks embedded at the notch root were investigated using the finite element method (FEM). The anisotropic material properties were shown to have a significant effect on both the stress and strain distribution in the notch region and the crack-tip parameters. The results of the experimental study have shown that fatigue cracks formation occurs via expansion of elliptical subsurface interdendritic pores located at high stress regions in the notch. Once the subsurface crack intersected the notch surface, subsequent crack growth occurred as semi-elliptical surface cracks. The secondary crystallographic orientation had a marked effect on crack-initiation life (the number of cycles to form a crack with a surface length of 760 mum) but no effect on small crack propagation behaviour. Crack initiation life predictions were made using a holistic lifing approach that considers the size, distribution and local stresses acting at the subsurface pores and utilizes the small fatigue crack growth data obtained from the experimental study. The predictions were found to agree reasonably well with the experimental test results and to account for the crack initiation

  10. Effect of initial gamma prime size on the elevated temperature creep properties of single crystal nickel base superalloys

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.

    1987-01-01

    The influence of initial gamma-prime size and shape on the high-temperature creep properties of two single-crystal Ni-base superalloys was investigated. The two alloys were chosen to represent different magnitudes of gamma/gamma-prime lattice mismatch. A range of initial microstructures was produced by various quenching and aging treatments. Creep-rupture testing at 1000 C was performed under stresses where gamma-prime directionally coarsens to form gamma/gamma-prime lamellae in the early portion of the creep life. Both alloys exhibited a peak in creep resistance as a function of initial gamma-prime size. The peak corresponded to an initial microstructure consisting of cuboidal precipitates aligned along 001 line directions. These aligned cuboidal gamma-prime particles directionally coarsened into a relatively perfect lamellar gamma/gamma-prime structure in the early stages of creep, whereas the more irregularly shaped and distributed gamma-prime particles in both under- and overaged material formed more irregular lamellae with more imperfections. The alloy with a lower magnitude of mismatch was less sensitive to initial gamma-prime size and shape.

  11. Orientation and temperature dependence of some mechanical properties of the single-crystal nickel-base superalloy Rene N4. II - Low cycle fatigue behavior

    NASA Technical Reports Server (NTRS)

    Gabb, T. P.; Gayda, J.; Miner, R. V.

    1986-01-01

    The low cycle fatigue (LCF) properties of a single-crystal nickel-base superalloy Rene N4, have been examined at 760 and 980 C in air. Specimens having crystallographic orientations near the 001, 011, -111, 023, -236, and -145 lines were tested in fully reversed, total-strain-controlled LCF tests at a frequency of 0.1 Hz. At 760 C, this alloy exhibited orientation dependent tension-compression anisotropies of yielding which continued to failure. Also at 760 C, orientations exhibiting predominately single slip exhibited serrated yielding for many cycles. At 980 C, orientation dependencies of yielding behavior were smaller. In spite of the tension-compression anisotropies, cyclic stress range-strain range behavior was not strongly orientation dependent for either test temperature. Fatigue life on a total strain range basis was highly orientation dependent at 760 and 980 C and was related chiefly to elastic modulus, low modulus orientations having longer lives. Stage I crack growth on 111 planes was dominant at 760 C, while Stage II crack growth occurred at 980 C. Crack initiation generally occurred at near-surface micropores, but occasionally at oxidation spikes in the 980 C tests.

  12. Orientation and temperature dependence of some mechanical properties of the single-crystal nickel-base superalloy Rene N4. I - Tensile behavior

    NASA Technical Reports Server (NTRS)

    Miner, R. V.; Gayda, J.; Gabb, T. P.; Voigt, R. C.

    1986-01-01

    Single crystal specimens of a nickel-base superalloy with axes near 001, 011, and -112 were tested in tension at room temperature, 760, and 980 C. The alloy Rene N-4, 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, (all in weight percent). Analysis of slip band traces, specimen axis rotation, and dislocation Burgers vectors showed that at 760 and 980 C primary cube slip supplanted normal octahedral slip for the -112 line-oriented specimens. The other two orientations, which have lower resolved shear stresses on the cube system, exhibited octahedral slip at all three temperatures. The critical resolved shear stress is considerably greater on the cube system than on the octahedral system at room temperature. However, at 760 and 980 C the critical resolved shear stresses on the two systems are about the same. While the room temperature and 980 C yield strengths for the two orientations exhibiting octahedral slip could be rationalized on the basis of resolved shear stress, those at 760 C could not. Such violations of Schmid's law have previously been observed in other superalloys and single phase gamma-prime.

  13. The effect of hydrogen and microstructure on the deformation and fracture behavior of a single crystal nickel-base superalloy. Final Report Ph.D. Thesis

    NASA Technical Reports Server (NTRS)

    Walston, William S.

    1990-01-01

    A study was conducted on the effects of internal hydrogen and microstructure on the deformation and fracture of a single crystal nickel-base superalloy. In particular, room temperature plane strain fracture toughness and tensile tests were performed on hydrogen-free and hydrogen charged samples of PWA 1480. The role of microstructure was incorporated by varying the levels of porosity and eutectic gamma/gamma prime through hot isostatic pressing and heat treatment. The room temperature behavior of PWA 1480 was unusual because precipitate shearing was not the primary deformation mechanism at all strains. At strains over 1 percent, dislocations were trapped in the gamma matrix and an attempt was made to relate this behavior to compositional differences between PWA 1480 and other superalloys. Another unique feature of the tensile behavior was cleavage of the eutectic gamma/gamma prime, which is believed to initiate the failure process. Fracture occurred on (111) planes and is likely a result of shear localization along these planes. Elimination of the eutectic gamma/gamma prime greatly improved the tensile ductility, but pososity had no effect on tensile properties. Large quantities of hydrogen (1.74 at. percent) were gas-phase charged into the material, but surprisingly this was not a function of the amount of porosity or eutectic gamma/gamma prime present. Desorption experiments suggest that the vast majority of hydrogen is at reversible lattice trapping sites. This large, uniform concentration of hydrogen dramatically reduced the tensile strain to failure, but only slightly affected the reduction in area. Available hydrogen embrittlement models were examined in light of these results and it was found that the hydrogen enhanced localized plasticity model can explain much of the tensile behavior. K(IC) fracture toughness tests were conducted, but it was necessary to also perform J(IC) tests to provide valid data.

  14. Detailed Analysis of the Solution Heat Treatment of a Third-Generation Single-Crystal Nickel-Based Superalloy CMSX-10K®

    NASA Astrophysics Data System (ADS)

    Pang, Hon Tong; D'Souza, Neil; Dong, Hongbiao; Stone, Howard J.; Rae, Catherine M. F.

    2016-02-01

    A detailed analysis of the response of as-cast third-generation single-crystal nickel-based superalloy CMSX-10K® to solution heat treatment (SHT) has been carried out, alongside an SHT optimization exercise. The analysis was conducted through microstructural characterization, differential scanning calorimetry, and compositional homogeneity measurements, quantifying (i) the dissolution and microstructural evolution of the inter-dendritic constituents, (ii) the shift in thermo-physical characteristics of the material, and (iii) the change in compositional homogeneity across the microstructure, in order to gain further understanding of these phenomena during the progression of the SHT. During the early stages of SHT, the coarse cellular γ'/narrow γ channel inter-dendritic constituents which were the last areas to solidify during casting, progressively dissolve; homogenization between these inter-dendritic areas and adjacent dendritic areas leads to a rapid increase in the incipient melting temperature T IM. The fine γ/γ' morphology which were the first inter-dendritic constituents to solidify after primary γ dendrite solidification were found to progressively coarsen; however, subsequent dissolution of these coarsened γ/γ' inter-dendritic areas did not result in significant increases in the T IM until the near-complete dissolution of these inter-dendritic areas. After the final SHT step, residual compositional micro-segregation could still be detected across the microstructure despite the near-complete dissolution of these remnant inter-dendritic areas; even so the T IM of the material approached the solidus temperature of the alloy.

  15. Phase-contrast x-ray imaging of microstructure and fatigue-crack propagation in single-crystal nickel-base superalloys

    NASA Astrophysics Data System (ADS)

    Husseini, Naji Sami

    Single-crystal nickel-base superalloys are ubiquitous in demanding turbine-blade applications, and they owe their remarkable resilience to their dendritic, hierarchical microstructure and complex composition. During normal operations, they endure rapid low-stress vibrations that may initiate fatigue cracks. This failure mode in the very high-cycle regime is poorly understood, in part due to inadequate testing and diagnostic equipment. Phase-contrast imaging with coherent synchrotron x rays, however, is an emergent technique ideally suited for dynamic processes such as crack initiation and propagation. A specially designed portable ultrasonic-fatigue apparatus, coupled with x-ray radiography, allows real-time, in situ imaging while simulating service conditions. Three contrast mechanisms - absorption, diffraction, and phase contrast - span the immense breadth of microstructural features in superalloys. Absorption contrast is sensitive to composition and crack displacements, and diffraction contrast illuminates dislocation aggregates and crystallographic misorientations. Phase contrast enhances electron-density gradients and is particularly useful for fatigue-crack studies, sensitive to internal crack tips and openings less than one micrometer. Superalloy samples were imaged without external stresses to study microstructure and mosaicity. Maps of rhenium and tungsten concentrations revealed strong segregation to the center of dendrites, as manifested by absorption contrast. Though nominally single crystals, dendrites were misoriented from the bulk by a few degrees, as revealed by diffraction contrast. For dynamic studies of cyclic fatigue, superalloys were mounted in the portable ultrasonic-fatigue apparatus, subjected to a mean tensile stress of ˜50-150 MPa, and cycled in tension to initiate and propagate fatigue cracks. Radiographs were recorded every thousand cycles over the multimillion-cycle lifetime to measure micron-scale crack growth. Crack

  16. 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.

  17. The influence of high thermal gradient casting, hot isostatic pressing and alternate heat treatment on the structure and properties of a single crystal nickel base superalloy

    NASA Technical Reports Server (NTRS)

    Fritzemeier, L. G.

    1988-01-01

    A development program has been conducted to improve the cyclic properties of the PWA 1480 single-crystal superalloy by reducing or entirely eliminating casting porosity at fatigue-initiation sites, through the use of improved casting process parameters and HIPing; potential mechanical property improvements in a high-pressure hydrogen environment were also sought in alternatives to the standard coating and heat-treatment cycle. High thermal gradient casting was found to yield a reduction in overall casting porosity density and pore sizes. The most dramatic mechanical property improvement resulted from HIPing.

  18. Morphological changes of gamma prime precipitates in nickel-base superalloy single crystals. Ph.D. Thesis - Case Western Reserve Univ., May 1984

    NASA Technical Reports Server (NTRS)

    Mackay, R. A.

    1984-01-01

    Changes in the morphology of the gamma prime precipitate were examined during tensile creep at temperatures between 927 and 1038 C in 001-oriented single crystals of a Ni-Al-Mo-Ta superalloy. In this alloy, which has a large negative misfit of -0.80%, the gamma prime particles link together during creep to form platelets, or rafts, which are aligned with their broad faces perpendicular to the applied tensile axis. The dimensions of the gamma and gamma prime phases were measured as directional coarsening developed in an attempt to trace the changing morphology under various stress levels. In addition, the effects of initial microstructure, as well as slight compositional variations, were related to raft development and creep properties. The results showed that directional coarsening of gamma prime began during primary creep, and under certain conditions, continued to develop after the onset of steady-state creep. The length of the rafts increased linearly with time up to a plateau region. The thickness of the rafts, however, remained equal to the initial gamma prime size at least up through the onset of tertiary creep; this is a clear indication of the stability of the finely-spaced gamma-gamma prime lamellar structure. It was found that the single crystals with the finest gamma prime size exhibited the longest creep lives, because the resultant rafted structure had a larger number of gamma-gamma prime interfaces per unit volume of material.

  19. Single-crystal nickel-based superalloys developed by numerical multi-criteria optimization techniques: design based on thermodynamic calculations and experimental validation

    NASA Astrophysics Data System (ADS)

    Rettig, Ralf; Ritter, Nils C.; Helmer, Harald E.; Neumeier, Steffen; Singer, Robert F.

    2015-04-01

    A method for finding the optimum alloy compositions considering a large number of property requirements and constraints by systematic exploration of large composition spaces is proposed. It is based on a numerical multi-criteria global optimization algorithm (multistart solver using Sequential Quadratic Programming), which delivers the exact optimum considering all constraints. The CALPHAD method is used to provide the thermodynamic equilibrium properties, and the creep strength of the alloys is predicted based on a qualitative numerical model considering the solid solution strengthening of the matrix by the elements Re, Mo and W and the optimum morphology and fraction of the γ‧-phase. The calculated alloy properties which are required as an input for the optimization algorithm are provided via very fast Kriging surrogate models. This greatly reduces the total calculation time of the optimization to the order of minutes on a personal computer. The capability of the multi-criteria optimization method developed was experimentally verified with two new single crystal superalloys. Their compositions were designed such that the content of expensive elements was reduced. One of the newly designed alloys, termed ERBO/13, is found to possess creep strength of only 14 K below CMSX-4 in the high-temperature/low-stress regime although it is a Re-free alloy.

  20. The effect of tantalum and carbon on the structure/properties of a single crystal nickel-base superalloy. M.S. Thesis. Final Report

    NASA Technical Reports Server (NTRS)

    Nguyen, H. C.

    1984-01-01

    The microstructure, phase chemistry, and creep and hot tensile properties were studied as a function of tantalum and carbon levels in Mar-M247 type single crystal alloys. Microstructural studies showed that several types of carbides (MC, M23C6 and M5C) are present in the normal carbon (0.10 wt % C) alloys after heat treatment. In general, the composition of the MC carbides changes from titanium rich to tantalum rich as the tantalum level in the alloy increases. Small M23C6 carbides are present in all alloys. Tungsten rich M6C carbides are also observed in the alloy containing no tantalum. No carbides are present in the low carbon (0.01 wt % C) alloy series. The morphology of gamma prime is observed to be sensitive to heat treatment and tantalum level in the alloy. Cuboidal gamma prime is present in all the as cast structures. After heat treatment, the gamma prime precipitates tend to have a more spheroidal like morphology, and this tendency increases as the tantalum level decreases. On prolonged aging, the gamma prime reverts back to a cuboidal morphology or under stress at high temperatures, forms a rafted structure. The weight fraction and lattice parameter of the spheroidal gamma prime increases with increasing tantalum content. Changes in the phase chemistry of the gamma prime matrix and gamma prime have also been analyzed using phase extraction techniques. The partitioning ratio decreases for tungsten and aluminum and increases for tantalum as the tantalum content increases for both alloy series; no significant changes occur in the partitioning ratios of the other alloying elements. A reduction in secondary creep rate and an increase in rupture time result from increasing the tantalum content and decreasing the carbon level.

  1. The key role of dislocation dissociation in the plastic behaviour of single crystal nickel-based superalloy with low stacking fault energy: Three-dimensional discrete dislocation dynamics modelling

    NASA Astrophysics Data System (ADS)

    Huang, Minsheng; Li, Zhenhuan

    2013-12-01

    To model the deformation of single crystal nickel based superalloys (SCNBS) with low stacking fault energy (SFE), three-dimensional discrete dislocation dynamics (3D-DDD) is extended by incorporating dislocation dissociation mechanism. The present 3D-DDD simulations show that, consistent with the existing TEM observation, the leading partial can enter the matrix channel efficiently while the trailing partial can hardly glide into it when the dislocation dissociation is taken into account. To determine whether the dislocation dissociation can occur or not, a critical percolation stress (CPS) based criterion is suggested. According to this CPS criterion, for SCNBS there exists a critical matrix channel width. When the channel width is lower than this critical value, the dislocation tends to dissociate into an extended configuration and vice versa. To clarify the influence of dislocation dissociation on CPS, the classical Orowan formula is improved by incorporating the SFE. Moreover, the present 3D-DDD simulations also show that the yielding stress of SCNBSs with low SFE may be overestimated up to 30% if the dislocation dissociation is ignored. With dislocation dissociation being considered, the size effect due to the width of γ matrix channel and the length of γ‧ precipitates on the stress-strain responses of SCNBS can be enhanced remarkably. In addition, due to the strong constraint effect by the two-phase microstructure in SCNBS, the configuration of formed junctions is quite different from that in single phase crystals such as Cu. The present results not only provide clear understanding of the two-phase microstructure levelled microplastic mechanisms in SCNBSs with low SFE, but also help to develop new continuum-levelled constitutive laws for SCNBSs.

  2. In Situ Measurement of the γ/ γ' Lattice Mismatch Evolution of a Nickel-Based Single-Crystal Superalloy During Non-isothermal Very High-Temperature Creep Experiments

    NASA Astrophysics Data System (ADS)

    Le Graverend, Jean-Briac; Dirand, Laura; Jacques, Alain; Cormier, Jonathan; Ferry, Olivier; Schenk, Thomas; Gallerneau, Franck; Kruch, Serge; Mendez, José

    2012-11-01

    The evolution of the γ/ γ' lattice mismatch of the AM1 single-crystal superalloy was measured during in situ non-isothermal very high-temperature creep tests under X-ray synchrotron radiation. The magnitude of the effective lattice mismatch in the 1273 K to 1323 K (1000 °C to 1050 °C) temperature range always increased after overheatings performed at temperatures lower than 1403 K (1130 °C). In contrast, a decrease of its magnitude was observed after overheatings at temperatures greater than 1453 K (1180 °C) due to massive dislocation recovery processes occurring at very high temperature.

  3. Dendritic growth and crystalline quality of nickel-base single grains

    NASA Astrophysics Data System (ADS)

    Siredey, Nathalie; Boufoussi, M'Bareck; Denis, Sabine; Lacaze, Jacques

    1993-05-01

    It is a usual observation that subgrains exist in nickel-base single grain components solidified by the lost wax process. The associated misorientations are generally small, but they can eventually lead to casting defects in the case of highly complex mold shapes. This work presents an attempt to relate the formation of subgrain boundaries with the development of the dendritic solidification microstructure. Experimental investigations have been undertaken on cast components made of AM1 nickel-base superalloy designed for high temperature turbine blades. Single grains were obtained by means of a grain selector at the bottom of each part. Metallographic observations have been made to characterize the dendritic array, together with gamma diffraction to measure the crystalline quality of the material and X-ray topography for mapping of misorientations on a dendritic scale. Small misorientations between dendrite stems have been found at the upper end of the selector which lead to the formation of subgrains. Moreover, during the growth process, the total mosaicity of the material increases, firstly as a consequence of an increase in the misorientations between subgrains, and secondly because of a decrease of the internal quality of each subgrain. It is proposed that misorientations are due to thermomechanical stresses which build up during λ' precipitation at temperatures slightly below the solidus temperature of the alloy.

  4. Development of a hydrogen-based annealing process for desulfurization of single crystalline, nickel-based superalloy. Final report

    SciTech Connect

    Smith, M.; Mickle, T.H.; Frazier, W.E.; Waldman, J.

    1994-11-05

    The presence of minor amounts of sulfur (1-10 ppm) in nickel-based superalloys has been associated with reduced oxidation resistance and premature spallation of protective coatings. A hydrogen annealing process has been developed by NAWCADWAR which effectively reduces the sulfur content of superalloys. The conditions which allow effective desulfurization are delineated. Diffusion of sulfur through the superalloy is found to be the rate controlling step for the process.

  5. Constitutive Modeling of Superalloy Single Crystals and Directionally Solidified Materials

    NASA Technical Reports Server (NTRS)

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

    1985-01-01

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

  6. Fatigue damage modeling for coated single crystal superalloys

    NASA Technical Reports Server (NTRS)

    Nissley, David M.

    1988-01-01

    A high temperature, low-cycle fatigue life prediction method for coated single crystal nickel-base superalloys is being developed. The method is being developed for use in predicting crack initiation life of coated single crystal turbine airfoils. Although the models are being developed using coated single crystal PWA 1480, they should be readily adaptable to other coated nickel-base single crystal materials. The coatings choosen for this effort were of two generic types: a low pressure plasma sprayed NiCoCrAlY overlay, designated PWA 286, and an aluminide diffusion, designated PWA 273. In order to predict the useful crack initiation life of airfoils, the constitutive and failure behavior of the coating/substrate combination must be taken into account. Coatings alter the airfoil surface microstructure and are a primary source from which cracks originate. The adopted life prediction approach addresses this complexity by separating the coating and single crystal crack initiation regimes. This provides a flexible means for using different life model formulations for the coating and single crystal materials. At the completion of this program, all constitutive and life model formulations will be available in equation form and as software. The software will use the MARC general purpose finite element code to drive the constitutive models and calculate life parameters.

  7. 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.

  8. Hydrogen Annealing Of Single-Crystal Superalloys

    NASA Technical Reports Server (NTRS)

    Smialek, James L.; Schaeffer, John C.; Murphy, Wendy

    1995-01-01

    Annealing at temperature equal to or greater than 2,200 degrees F in atmosphere of hydrogen found to increase ability of single-crystal superalloys to resist oxidation when subsequently exposed to oxidizing atmospheres at temperatures almost as high. Supperalloys in question are principal constituents of hot-stage airfoils (blades) in aircraft and ground-based turbine engines; also used in other high-temperature applications like chemical-processing plants, coal-gasification plants, petrochemical refineries, and boilers. Hydrogen anneal provides resistance to oxidation without decreasing fatigue strength and without need for coating or reactive sulfur-gettering constituents. In comparison with coating, hydrogen annealing costs less. Benefits extend to stainless steels, nickel/chromium, and nickel-base alloys, subject to same scale-adhesion and oxidation-resistance considerations, except that scale is chromia instead of alumina.

  9. Single-crystal superalloy drives turbine advances

    SciTech Connect

    Harris, K.

    1995-04-01

    In searching for ways to improve power-to-weight ratios and fuel efficiency, gas turbine engine manufacturers invest heavily in the development and testing of new alloys. Their goal is to find turbine airfoil materials that can handle the higher operating temperatures, increased component stresses, and faster rotational speeds that are needed to increase turbine performance. Major turbine engine manufacturers find they can achieve these objectives through ultra-high performance, single-crystal superalloys -- a group of nickel-base materials that exhibit outstanding strength and surface stability at temperatures up to 85{percent} of their melting points. One such superalloy is CMSX-4, co-engineered by ingot maker Cannon-Muskegon and turbine engine manufacturers Rolls-Royce and Allison Engine Company. It is currently being used in such applications as Allison`s advanced airfoil programs.

  10. Fretting Stresses in Single Crystal Superalloy Turbine Blade Attachments

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Swanson, Gregory

    2000-01-01

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

  11. Constitutive modeling for single crystal superalloys

    NASA Technical Reports Server (NTRS)

    Stouffer, D. C.; Jayaraman, N.; Sheh, M.; Alden, D.

    1986-01-01

    The inelastic response of single crystal gamma/gamma prime superalloys is quite different from the behavior of polycrystalline nickel base superalloys. Upto a critical temperature the yield stress of single crystal alloys is a function of the material orientation relative to the direction of the applied stress and the material exhibits significant tension/compression asymmetry. This behavior is primarily due to slip on the octahedral slip system. Above the critical temperature there is a sharp drop in the yield stress, cube slip becomes more predominant and the tension/compression asymmetry is reduced. Similar orientation and tension/compression asymmetry is observed in creep and secondary creep above the critical temperature is inferred to occur by octahedral slip. There are two exceptions to this behavior. First, loading near the (111) orientation exhibits cube slip at all temperatures, and; second, loading near the (001) orientation produces only octahedral slip at all temperatures. The constitutive model is based on separating the total global strain into elastic and inelastic components. This model is developed and briefly discussed.

  12. NICKEL-BASE ALLOY

    DOEpatents

    Inouye, H.; Manly, W.D.; Roche, T.K.

    1960-01-19

    A nickel-base alloy was developed which is particularly useful for the containment of molten fluoride salts in reactors. The alloy is resistant to both salt corrosion and oxidation and may be used at temperatures as high as 1800 deg F. Basically, the alloy consists of 15 to 22 wt.% molybdenum, a small amount of carbon, and 6 to 8 wt.% chromium, the balance being nickel. Up to 4 wt.% of tungsten, tantalum, vanadium, or niobium may be added to strengthen the alloy.

  13. 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.

  14. Bioengineering single crystal growth.

    PubMed

    Wu, Ching-Hsuan; Park, Alexander; Joester, Derk

    2011-02-16

    Biomineralization is a "bottom-up" synthesis process that results in the formation of inorganic/organic nanocomposites with unrivaled control over structure, superior mechanical properties, adaptive response, and the capability of self-repair. While de novo design of such highly optimized materials may still be out of reach, engineering of the biosynthetic machinery may offer an alternative route to design advanced materials. Herein, we present an approach using micro-contact-printed lectins for patterning sea urchin embryo primary mesenchyme cells (PMCs) in vitro. We demonstrate not only that PMCs cultured on these substrates show attachment to wheat germ agglutinin and concanavalin A patterns but, more importantly, that the deposition and elongation of calcite spicules occurs cooperatively by multiple cells and in alignment with the printed pattern. This allows us to control the placement and orientation of smooth, cylindrical calcite single crystals where the crystallographic c-direction is parallel to the cylinder axis and the underlying line pattern. PMID:21265521

  15. Advanced single crystal for SSME turbopumps

    NASA Technical Reports Server (NTRS)

    Fritzemeier, L. G.

    1989-01-01

    The objective of this program was to evaluate the influence of high thermal gradient casting, hot isostatic pressing (HIP) and alternate heat treatments on the microstructure and mechanical properties of a single crystal nickel base superalloy. The alloy chosen for the study was PWA 1480, a well characterized, commercial alloy which had previously been chosen as a candidate for the Space Shuttle Main Engine high pressure turbopump turbine blades. Microstructural characterization evaluated the influence of casting thermal gradient on dendrite arm spacing, casting porosity distribution and alloy homogeneity. Hot isostatic pressing was evaluated as a means of eliminating porosity as a preferred fatigue crack initiation site. The alternate heat treatment was chosen to improve hydrogen environment embrittlement resistance and for potential fatigue life improvement. Mechanical property evaluation was aimed primarily at determining improvements in low cycle and high cycle fatigue life due to the advanced processing methods. Statistically significant numbers of tests were conducted to quantitatively demonstrate life differences. High thermal gradient casting improves as-cast homogeneity, which facilitates solution heat treatment of PWA 1480 and provides a decrease in internal pore size, leading to increases in low cycle and high cycle fatigue lives.

  16. The evaluation of single crystal superalloys for turbopump blades in the SSME

    NASA Technical Reports Server (NTRS)

    Bowen, K.; Nagy, P.; Parr, R. A.

    1986-01-01

    This paper discusses single-crystal nickel-base superalloys for use in gaseous hydrogen environments, like the Space Shuttle Main Engine (SSME). PWA 1480E was chosen as a candidate alloy based on strength retention in hydrogen environments. Selection of single-crystal-alloy primary and secondary crystallographic axes allows tailoring of the airfoil resonant frequency as a function of orientation. PWA 1480E 111-line primary orientation proved to be the most hydrogen-resistant orientation. By choosing the proper primary and secondary orientation combinations, the fourth excitation mode of the SSME may be avoided.

  17. Elastic response of zone axis (001)-oriented PWA 1480 single crystal: The influence of secondary orientation

    NASA Technical Reports Server (NTRS)

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

    1991-01-01

    The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

  18. Subsurface Stress Fields In Single Crystal (Anisotropic) Contacts

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Knudsen, Erik C.; Duke, Greg; Battista, Gilda; Swanson, Greg

    2004-01-01

    Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and alternating stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent HCF failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and noncrystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. This paper presents analytical and numerical techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts. The subsurface stress results are required for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades. An analytical procedure is , presented, for evaluating the subsurface stresses in the elastic half-space, using a complex potential method outlined by Lekhnitskii. Numerical results are presented for cylindrical and spherical anisotropic contacts, using finite element analysis. Effects of crystal orientation on stress response and fatigue life are examined.

  19. Wave propagation in an anisotropic nickel-based superalloy

    PubMed

    Amulele; Every

    2000-03-01

    The effects of elastic anisotropy on ultrasound propagation in a nickel-based single crystal test component are studied using a 25 MHz focused probe in a water immersion system. Anisotropy gives rise to directionally dependent acoustic wavespeeds, beam steering, acoustic energy focusing and mode conversion for normal incidence. Transverse mode echoes are particularly strong in the vicinity of crystallographic directions in which the Gaussian curvature of the slowness surface is zero and divergence of the echo amplitude is predicted on the basis of the stationary phase approximation. There are other directions where the transverse mode echoes vanish for symmetry reasons. The longitudinal mode echo amplitude also shows significant variation with direction. Overall there is good agreement between the echo signal arrival times and amplitudes we measure and calculation. Progress in applying this technique to gas turbine blades is reported. PMID:10829669

  20. Niobium enrichment and environmental enhancement of creep crack growth in nickel-base superalloys

    SciTech Connect

    Gao, M.; Wei, R.P.; Dwyer, D.J.

    1995-04-15

    In this paper, the possible role of niobium in the environmental enhancement of creep crack growth in nickel-base superalloys is further examined. The examination included (1) surface enrichment of Nb in a commercial Inconel 718; (2) a source of niobium and its interaction with oxygen; (3) preferential oxidation of Nb at the crack tip, and (4) correlations between environmental sensitivity and niobium concentration of nickel-base superalloys from the literature. The role of niobium was suggested by recent X-ray photoelectron spectroscopic (XPS) studies. The XPS studies show a significant increase in the concentration of niobium on the (001) surface of an Inconel 718 single crystal after heating at temperatures above 775 K. Considerable segregation of niobium was also found on the grain boundaries of a thermally aged commercial (polycrystalline) Inconel 718. The CCGR data showed significant enhancement by oxygen and water vapor at temperatures of 800--975 K where niobium enrichment occurred.

  1. Subsurface Stress Fields in Single Crystal (Anisotropic) Contacts

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.

    2003-01-01

    Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and fatigue stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent HCF failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and noncrystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. Techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts are presented in this report. Figure 1 shows typical damper contact locations in a turbine blade. The subsurface stress results are used for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades.

  2. Low cycle fatigue of MAR-M 200 single crystals at 760 and 870 deg C

    NASA Technical Reports Server (NTRS)

    Milligan, W. W.; Jayaraman, N.; Bill, R. C.

    1984-01-01

    Fully reversed low cycle fatigue tests were conducted on single crystals of the nickel-base superalloys Mar-M 200 at 760 C and 870 C. At 760 C, planar slip (octahedral) lead to orientation-dependent strain hardening and cyclic lives. Multiple slip crystals strain hardened the most, resulting in relatively high stress ranges and low lives. Single slip crystals strain hardened the least, resulting in relatively low stress ranges and higher lives. A preferential crack initiation site which was related to slip plane geometry was observed in single slip orientated crystals. At 870 C, the trends were quite different, and the slip character was much more homogeneous. As the tensile axis orientation deviated from 001 , the stress ranges increased and the cyclic lives decreased. Two possible mechanisms were proposed to explain the behavior: one is based on Takeuchi and Kuramoto's cube cross-slip model, and the other is based on orientation-dependent creep rates.

  3. Development of single crystal membranes

    NASA Technical Reports Server (NTRS)

    Stormont, R. W.; Cocks, F. H.

    1972-01-01

    The design and construction of a high pressure crystal growth chamber was accomplished which would allow the growth of crystals under inert gas pressures of 2 MN/sq m (300 psi). A novel crystal growth technique called EFG was used to grow tubes and rods of the hollandite compounds, BaMgTi7O16, K2MgTi7O16, and tubes of sodium beta-alumina, sodium magnesium-alumina, and potassium beta-alumina. Rods and tubes grown are characterized using metallographic and X-ray diffraction techniques. The hollandite compounds are found to be two or three-phase, composed of coarse grained orientated crystallites. Single crystal c-axis tubes of sodium beta-alumina were grown from melts containing excess sodium oxide. Additional experiments demonstrated that crystals of magnesia doped beta-alumina and potassium beta-alumina also can be achieved by this EFG technique.

  4. Mechanisms of High Temperature/Low Stress Creep of Ni-Based Superalloy Single Crystals

    SciTech Connect

    Michael J. Mills

    2009-03-05

    Cast nickel-based superalloys are used for blades in land-based, energy conversion and powerplant applications, as well as in aircraft gas turbines operating at temperatures up to 1100 C, where creep is one of the life-limiting factors. Creep of superalloy single crystals has been extensively studied over the last several decades. Surprisingly, only recently has work focused specifically on the dislocation mechanisms that govern high temperature and low stress creep. Nevertheless, the perpetual goal of better engine efficiency demands that the creep mechanisms operative in this regime be fully understood in order to develop alloys and microstructures with improved high temperature capability. At present, the micro-mechanisms controlling creep before and after rafting (the microstructure evolution typical of high temperature creep) has occurred have yet to be identified and modeled, particularly for [001] oriented single crystals. This crystal orientation is most interesting technologically since it exhibits the highest creep strength. The major goal of the program entitled ''Mechanisms of High Temperature/Low Stress Creep of Ni-Based Superalloy Single Crystals'' (DOE Grant DE-FG02-04ER46137) has been to elucidate these creep mechanisms in cast nickel-based superalloys. We have utilized a combination of detailed microstructure and dislocation substructure analysis combined with the development of a novel phase-field model for microstructure evolution.

  5. Subsurface Stress Fields in FCC Single Crystal Anisotropic Contacts

    NASA Technical Reports Server (NTRS)

    Arakere, Nagaraj K.; Knudsen, Erik; Swanson, Gregory R.; Duke, Gregory; Ham-Battista, Gilda

    2004-01-01

    Single crystal superalloy turbine blades used in high pressure turbomachinery are subject to conditions of high temperature, triaxial steady and alternating stresses, fretting stresses in the blade attachment and damper contact locations, and exposure to high-pressure hydrogen. The blades are also subjected to extreme variations in temperature during start-up and shutdown transients. The most prevalent high cycle fatigue (HCF) failure modes observed in these blades during operation include crystallographic crack initiation/propagation on octahedral planes, and non-crystallographic initiation with crystallographic growth. Numerous cases of crack initiation and crack propagation at the blade leading edge tip, blade attachment regions, and damper contact locations have been documented. Understanding crack initiation/propagation under mixed-mode loading conditions is critical for establishing a systematic procedure for evaluating HCF life of single crystal turbine blades. This paper presents analytical and numerical techniques for evaluating two and three dimensional subsurface stress fields in anisotropic contacts. The subsurface stress results are required for evaluating contact fatigue life at damper contacts and dovetail attachment regions in single crystal nickel-base superalloy turbine blades. An analytical procedure is presented for evaluating the subsurface stresses in the elastic half-space, based on the adaptation of a stress function method outlined by Lekhnitskii. Numerical results are presented for cylindrical and spherical anisotropic contacts, using finite element analysis (FEA). Effects of crystal orientation on stress response and fatigue life are examined. Obtaining accurate subsurface stress results for anisotropic single crystal contact problems require extremely refined three-dimensional (3-D) finite element grids, especially in the edge of contact region. Obtaining resolved shear stresses (RSS) on the principal slip planes also involves

  6. The Effects of Stress Triaxiality, Temperature and Strain Rate on the Fracture Characteristics of a Nickel-Base Superalloy

    NASA Astrophysics Data System (ADS)

    Wang, Jianjun; Guo, Weiguo; Guo, Jin; Wang, Ziang; Lu, Shengli

    2016-05-01

    In this work, to study the effects of stress triaxiality, temperature, and strain rate on the fracture behaviors of a single-crystal Nickel-base superalloy, a series of experiments over a temperature range of 293 to 1373 K, strain rate range of 0.001 to 4000/s, and stress triaxiality range of -0.6 to 1.1 are conducted. Anomalous peak of stress is noticed in the yield stress versus temperature curves, and strain rate effect on the anomalous peak of yield stress is analyzed. The anomalous peak shifts to higher temperature as the strain rate increases. Then the effects of stress triaxiality, temperature, and strain rate on its fracture behaviors, including strain to fracture, path of crack propagation, and fracture surface, are observed and analyzed. A valley of the fracture strain is formed in the fracture strain versus temperature curve over the selected temperature range. The micrograph of fracture surface is largely dependent on the temperature, stress triaxiality, and strain rate. Finally, the original Johnson-Cook (J-C) fracture criterion cannot describe the effect of stress triaxiality and temperature on the fracture behaviors of single-crystal Nickel-base superalloy. A modified J-C fracture criterion is developed, which takes the anomalous stress triaxiality and temperature effects on the fracture behaviors of single-crystal Nickel-base superalloy into account.

  7. Stacking fault energy in some single crystals

    NASA Astrophysics Data System (ADS)

    Vora, Aditya M.

    2012-06-01

    The stacking fault energy of single crystals has been reported using the peak shift method. Presently studied all single crystals are grown by using a direct vapor transport (DVT) technique in the laboratory. The structural characterizations of these crystals are made by XRD. Considerable variations are shown in deformation (α) and growth (β) probabilities in single crystals due to off-stoichiometry, which possesses the stacking fault in the single crystal.

  8. A concept for the EQ coating system for nickel-based superalloys

    NASA Astrophysics Data System (ADS)

    Kawagishi, K.; Sato, A.; Harada, H.

    2008-07-01

    Nickel-based single-crystal superalloys with high concentrations of refractory elements are prone to generate a diffusion layer called a secondary reaction zone (SRZ) beneath their bond coating during long exposure to high temperatures. The SRZ causes a reduction of the load-bearing cross section and it is detrimental to the creep properties of thin-walled turbine airfoils. In this study, a new bond coat system, “EQ coating,” which is thermodynamically stable and suppresses SRZ has been proposed. Diffusion couples of coating materials and substrate alloys were made and heat treated at 1,100°C for 300 h and 1,000 h. Cyclic oxidation examinations were carried out at 1,100°C in air and the oxidation properties of EQ coating materials were discussed. High-velocity frame-sprayed EQ coatings designed for second-generation nickel-based superalloys were deposited on fourth-and fifth-generation nickel-based superalloys, and the stability of the microstructure at the interface and creep property of the coating system were investigated.

  9. Gamma prime shape changes during creep of a nickel-base superalloy

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Ebert, L. J.

    1983-01-01

    Changes in the shape of the gamma-prime phase in the single-crystal nickel base alloy NASAIR 100 during tensile and compressive creep have been investigated experimentally by Laue X-ray diffractometry. It is found that under tensile loading, gamma-prime changes from the initial cubic shape to plates perpendicular to the applied stress. This change occurs during primary creep at 1000 C, 148 MPa. Prolonged creep exposures result in a thickening of the gamma-prime plates that is similar to Ostwald ripening often observed in other superalloys during creep. Under compressive loading, two sets of gamma-prime plates parallel to the applied stress are formed.

  10. Elevated temperature fretting fatigue of nickel based alloys

    NASA Astrophysics Data System (ADS)

    Gean, Matthew C.

    This document details the high temperature fretting fatigue of high temperature nickel based alloys common to turbine disk and blade applications. The research consists of three area of focus: Experiments are conducted to determine quantitatively the fretting fatigue lives of advanced nickel based alloys; Analytical tools are developed and used to investigate the fretting fatigue response of the material; Fractographic analysis of the experimental results is used to improve the analytical models employed in the analysis of the experiments. Sixty three fretting fatigue experiments were conducted at 649 °C using a polycrystalline Nickel specimen in contact with directionally solidified and single crystal Nickel pads. Various influences on the fretting fatigue life are investigated. Shot peened Rene' 95 had better fretting fatigue life compared to shot peened Rene' 88. Shot peening produced a 2x increase in life for Rene' 95, but only a marginal improvement in the fretting fatigue life for Rene' 88. Minor cycles in variable amplitude loading produces significant damage to the specimen. Addition of occasional overpeaks in load produces improvements in fretting fatigue life. Contact tractions and stresses are obtained through a variety of available tools. The contact tractions can be efficiently obtained for limited geometries, while FEM can provide the contact tractions for a broader class of problems, but with the cost of increased CPU requirements. Similarly, the subsurface contact stresses can be obtained using the contact tractions as a boundary condition with either a semi-analytical FFT method or FEM. It is found that to calculate contact stresses the FFT was only marginally faster than FEM. The experimental results are combined with the analysis to produce tools that are used to design against fretting fatigue. Fractographic analysis of the fracture surface indicates the nature of the fretting fatigue crack behavior. Interrupted tests were performed to analyze

  11. Titania single crystals with a curved surface

    NASA Astrophysics Data System (ADS)

    Yang, Shuang; Yang, Bing Xing; Wu, Long; Li, Yu Hang; Liu, Porun; Zhao, Huijun; Yu, Yan Yan; Gong, Xue Qing; Yang, Hua Gui

    2014-11-01

    Owing to its scientific and technological importance, crystallization as a ubiquitous phenomenon has been widely studied over centuries. Well-developed single crystals are generally enclosed by regular flat facets spontaneously to form polyhedral morphologies because of the well-known self-confinement principle for crystal growth. However, in nature, complex single crystalline calcitic skeleton of biological organisms generally has a curved external surface formed by specific interactions between organic moieties and biocompatible minerals. Here we show a new class of crystal surface of TiO2, which is enclosed by quasi continuous high-index microfacets and thus has a unique truncated biconic morphology. Such single crystals may open a new direction for crystal growth study since, in principle, crystal growth rates of all facets between two normal {101} and {011} crystal surfaces are almost identical. In other words, the facet with continuous Miller index can exist because of the continuous curvature on the crystal surface.

  12. Titania single crystals with a curved surface.

    PubMed

    Yang, Shuang; Yang, Bing Xing; Wu, Long; Li, Yu Hang; Liu, Porun; Zhao, Huijun; Yu, Yan Yan; Gong, Xue Qing; Yang, Hua Gui

    2014-01-01

    Owing to its scientific and technological importance, crystallization as a ubiquitous phenomenon has been widely studied over centuries. Well-developed single crystals are generally enclosed by regular flat facets spontaneously to form polyhedral morphologies because of the well-known self-confinement principle for crystal growth. However, in nature, complex single crystalline calcitic skeleton of biological organisms generally has a curved external surface formed by specific interactions between organic moieties and biocompatible minerals. Here we show a new class of crystal surface of TiO₂, which is enclosed by quasi continuous high-index microfacets and thus has a unique truncated biconic morphology. Such single crystals may open a new direction for crystal growth study since, in principle, crystal growth rates of all facets between two normal {101} and {011} crystal surfaces are almost identical. In other words, the facet with continuous Miller index can exist because of the continuous curvature on the crystal surface. PMID:25373513

  13. Nickel Base Superalloy Turbine Disk

    NASA Technical Reports Server (NTRS)

    Gabb, Timothy P. (Inventor); Gauda, John (Inventor); Telesman, Ignacy (Inventor); Kantzos, Pete T. (Inventor)

    2005-01-01

    A low solvus, high refractory alloy having unusually versatile processing mechanical property capabilities for advanced disks and rotors in gas turbine engines. The nickel base superalloy has a composition consisting essentially of, in weight percent, 3.0-4.0 N, 0.02-0.04 B, 0.02-0.05 C, 12.0-14.0 Cr, 19.0-22.0 Co, 2.0-3.5 Mo, greater than 1.0 to 2.1 Nb, 1.3 to 2.1 Ta,3.04.OTi,4.1 to 5.0 W, 0.03-0.06 Zr, and balance essentially Ni and incidental impurities. The superalloy combines ease of processing with high temperature capabilities to be suitable for use in various turbine engine disk, impeller, and shaft applications. The Co and Cr levels of the superalloy can provide low solvus temperature for high processing versatility. The W, Mo, Ta, and Nb refractory element levels of the superalloy can provide sustained strength, creep, and dwell crack growth resistance at high temperatures.

  14. Resonance ultrasound spectroscopy forward modeling and inverse characterization of nickel-based superalloys

    NASA Astrophysics Data System (ADS)

    Biedermann, Eric; Jauriqui, Leanne; Aldrin, John C.; Goodlet, Brent; Pollock, Tresa; Torbet, Chris; Mazdiyasni, Siamack

    2015-03-01

    The objective of this paper is to investigate Resonance Ultrasound Spectroscopy (RUS) measurement models to more precisely connect changes in the resonance frequencies of nickel-based super-alloy material to the macro/microscopic state. RUS models using analytical solutions and the finite element method (FEM) were developed to address varying elastic properties, grain structures and creep. Experimental studies were performed investigating the effect of exposure to high temperatures and stress for varying part shape and three grain structure classes: single crystals, directionally-solidified and polycrystalline structures. Inversion using both traditional analytical models was enhanced in order to simultaneously estimate varying material properties and changes in part geometry due to creep. Inversion using surrogate models from FEM simulations was also developed, addressing varying crystal orientation and complex geometries. Results are presented comparing the forward model trends and inversion results with nickel alloy parts under various test conditions.

  15. Single crystals for welding research

    SciTech Connect

    David, S.A.; Boatner, L.A.

    1991-01-01

    Most welds last for many years, but a few fail after a relatively short time. Knowing the reasons why welds fail is important because cracks in welds can threaten the safety of people in buildings, airplanes, ships, automobiles, and power plants. Bad welds can lead to costly, extended shutdowns of industrial facilities such as petroleum refineries. Thus, research on this very important fabrication technology is critical to the multibillion-dollar welding industry. Research at ORNL and elsewhere strives to determine the structural features that make some welds strong and others weak. The goals are to find cost-effective ways to characterize the structure and strength of a new weld, correctly predict whether it will last a long time, and determine the welding conditions most likely to produce high-quality welds. There is more to welding than meets the eye. The cracks that make welds fail result from the complexities of microstructures formed during welding. Thus weld microstructure is linked to weld properties such as mechanical strength. As the hot weld material cools from a liquid into a solid, the crystalline grains grow at different speeds and in different directions, forming a new microstructure. By using single crystals rather than polycrystalline alloys to study different weld microstructures, scientists at ORNL have developed a way to predict more accurately the microstructures of various welds. The results could guide welders in providing the right conditions (correct welding speed, heat input, and weld thickness) for producing safer, higher-quality, and longer-lasting welds.

  16. Ames Lab 101: Single Crystal Growth

    ScienceCinema

    Schlagel, Deborah

    2014-06-04

    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.

  17. Ames Lab 101: Single Crystal Growth

    SciTech Connect

    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.

  18. 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.

  19. Adhesion of single crystals on modified surfaces in crystallization fouling

    NASA Astrophysics Data System (ADS)

    Mayer, Moriz; Augustin, Wolfgang; Scholl, Stephan

    2012-12-01

    In crystallization fouling it has been observed that during a certain initial phase the fouling is formed by a non-uniform layer consisting of a population of single crystals. These single crystals are frequently formed by inverse soluble salts such as CaCO3. During heterogeneous nucleation and heterogeneous growth an interfacial area between the crystal and the heat transfer surface occurs. The development of this interfacial area is the reason for the adhesion of each single crystal and of all individual crystals, once a uniform layer has been built up. The emerging interfacial area is intrinsic to the heterogeneous nucleation of crystals and can be explained by the thermodynamic principle of the minimum of the Gibbs free energy. In this study CaCO3 crystals were grown heterogeneously on untreated and on modified surfaces inside a flow channel. An untreated stainless steel (AISI 304) surface was used as a reference. Following surface modifications were investigated: enameled and electropolished stainless steel as well as diamond-like-carbon based coatings on stainless steel substrate. The adhesion was measured through a novel measurement technique using a micromanipulator to shear off single crystals from the substrate which was fixed to a spring table inside a SEM.

  20. An Atomistic Simulation of Crack Propagation in a Nickel Single Crystal

    NASA Technical Reports Server (NTRS)

    Karimi, Majid

    2002-01-01

    The main objective of this paper is to determine mechanisms of crack propagation in a nickel single crystal. Motivation for selecting nickel as a case study is because we believe that its physical properties are very close to that of nickel-base super alloy. We are directed in identifying some generic trends that would lead a single crystalline material to failure. We believe that the results obtained here would be of interest to the experimentalists in guiding them to a more optimized experimental strategy. The dynamic crack propagation experiments are very difficult to do. We are partially motivated to fill the gap by generating the simulation results in lieu of the experimental ones for the cases where experiment can not be done or when the data is not available.

  1. Advanced piezoelectric single crystal based actuators

    NASA Astrophysics Data System (ADS)

    Jiang, Xiaoning; Rehrig, Paul W.; Hackenberger, Wesley S.; Smith, Edward; Dong, Shuxiang; Viehland, Dwight; Moore, Jim, Jr.; Patrick, Brian

    2005-05-01

    TRS is developing new actuators based on single crystal piezoelectric materials such as Pb(Zn1/3Nb2/3)1-xTixO3 (PZN-PT) and Pb(Mg1/3Nb2/3)x-1TixO3 (PMN-PT) which exhibit very high piezoelectric coefficients (d33 = 1800-2200 pC/N) and electromechanical coupling factors (k33 > 0.9), respectively, for a variety of applications, including active vibration damping, active flow control, high precision positioning, ultrasonic motors, deformable mirrors, and adaptive optics. The d32 cut crystal plate actuators showed d32 ~ -1600 pC/N, inter-digital electroded (IDE) plate actuators showed effective d33 ~ 1100 pC/N. Single crystal stack actuators with stroke of 10 μm-100 μm were developed and tested at both room temperature and cryogenic temperatures. Flextensional single crystal piezoelectric actuators with either stack driver or plate driver were developed with stroke 70 μm - > 250 μm. For large stroke cryogenic actuation (> 1mm), a single crystal piezomotor was developed and tested at temperature of 77 K-300K and stroke of > 10mm and step resolution of 20 nm were achieved. In order to demonstrate the significance of developed single crystal actuators, modeling on single crystal piezoelectric deformable mirrors and helicopter flap control using single crystal actuators were conducted and the modeling results show that more than 20 wavelength wavefront error could be corrected by using the single crystal deformable mirrors and +/- 5.8 ° flap deflection will be obtained for a 36" flap using single crystal stack actuators.

  2. Fatigue crack growth behavior of a single crystal alloy as observed through an in situ fatigue loading stage

    NASA Technical Reports Server (NTRS)

    Telesman, Jack; Kantzos, Peter

    1988-01-01

    An in situ fatigue loading stage inside a scanning electron microscope (SEM) was used to determine the fatigue crack growth behavior of a PWA 1480 single-crystal nickel-based superalloy. The loading stage permits real-time viewing of the fatigue damage processes at high magnification. The PWA 1480 single-crystal, single-edge notch specimens were tested with the load axis parallel to the (100) orientation. Two distinct fatigue failure mechanisms were identified. The crack growth rate differed substantially when the failure occurred on a single slip system in comparison to multislip system failure. Two processes by which crack branching is produced were identified and are discussed. Also discussed are the observed crack closure mechanisms.

  3. Fatique crack growth behavior of a single crystal alloy as observed through an in situ fatigue loading stage

    NASA Technical Reports Server (NTRS)

    Telesman, Jack; Kantzos, Peter

    1988-01-01

    An in situ fatigue loading stage inside a scanning electron microscope (SEM) was used to determine the fatigue crack growth behavior of a PWA 1480 single-crystal nickel-based superalloy. The loading stage permits real-time viewing of the fatigue damage processes at high magnification. The PWA 1480 single-crystal, single-edge notch specimens were tested with the load axis parallel to the (100) orientation. Two distinct fatigue failure mechanisms were identified. The crack growth rate differed substantially when the failure occurred on a single slip system in comparison to multislip system failure. Two processes by which crack branching is produced were identified and are discussed. Also discussed are the observed crack closure mechanisms.

  4. Single Crystal Sapphire Optical Fiber Sensor Instrumentation

    SciTech Connect

    Anbo Wang; Russell May; Gary R. Pickrell

    2000-10-28

    The goal of this 30 month program is to develop reliable accurate temperature sensors based on single crystal sapphire materials that can withstand the temperatures and corrosive agents present within the gasifier environment. The research for this reporting period has been segregated into two parallel paths--corrosion resistance measurements for single crystal sapphire fibers and investigation of single crystal sapphire sensor configurations. The ultimate goal of this phase one segment is to design, develop and demonstrate on a laboratory scale a suitable temperature measurement device that can be field tested in phase two of the program.

  5. Photocurrent multiplication in organic single crystals

    NASA Astrophysics Data System (ADS)

    Hiramoto, Masahiro; Miki, Ayako; Yoshida, Manabu; Yokoyama, Masaaki

    2002-08-01

    A photocurrent multiplication of up to 200 times has been observed in single crystals of naphthalene tetracarboxylic anhydride sandwiched between metal electrodes. Photocurrent multiplication arises from photoinduced electron injection occurring at the crystal/metal interface. The high-speed response of the multiplied photocurrent reached 500 ms.

  6. Aero engine test experience with CMSX-4{reg_sign} alloy single-crystal turbine blades

    SciTech Connect

    Fullagar, K.P.L.; Broomfield, R.W.; Hulands, M.; Harris, K.; Erickson, G.L.; Sikkenga, S.L.

    1996-04-01

    A team approach involving a turbine engine company (Rolls-Royce), its single-crystal casting facilities, and a superalloy developer and ingot manufacturer (Cannon-Muskegon), utilizing the concepts of simultaneous engineering, has been used to develop CMSX-4 alloy successfully for turbine blade applications. CMSX-4 alloy is a second-generation nickel-base single-crystal superalloy containing 3 percent (wt) rhenium (Re) and 70 percent volume fraction of the coherent {gamma}{prime} precipitate strengthening phase. The paper details the single-crystal casting process and heat treatment manufacturing development for turbine blades in CMSX-4 alloy. Competitive single-crystal casting yields are being achieved in production and extensive vacuum heat treatment experience confirms CMSX-4 alloy to have a practical production solution heat treat/homogenization ``window.`` The creep-rupture data-base on CMSX-4 alloy now includes 325 data points from 17 heats including 3,630 kg (8,000 lb) production size heats. An appreciable portion of this data was machined-from-blade (MFB) properties, which indicate turbine blade component capabilities based on single-crystal casting process, component configuration, and heat treatment. The use of hot isostatic pressing (HIP) has been shown to eliminate single-crystal casting micropores, which along with the essential absence of {gamma}/{gamma}{prime} eutectic phase, carbides, stable oxide, nitride and sulfide inclusions, results in remarkably high mechanical fatigue properties, with smooth and particularly notched specimens. The Re addition has been shown not only to benefit creep and mechanical fatigue strength, but also bare oxidation, hot corrosion, and coating performance. The high level of balanced properties determined by extensive laboratory evaluation has been confirmed during engine testing of the Rolls-Royce Pegasus turbofan.

  7. Temperature dependence of gamma-gamma prime lattice mismatch in nickel-base superalloys

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Mackay, R. A.; Garlick, R. G.

    1985-01-01

    High temperature X-ray diffraction techniques were used to determine the gamma-gamma prime lattice mismatch of three different nickel-base superalloys at temperatures between 18 and 1000 C. The measurements were performed on oriented single-crystal disks which had been aged to produce a semicoherent gamma-gamma prime structure. The thermal expansion of the lattice parameters of the gamma and gamma-prime phases was described by a second-order polynomial expression. The expansion of the gamma-prime phase was consistently smaller than that of the gamma phase, which caused the lattice mismatch to become more negative at higher temperatures. It was also shown that high values of lattice mismatch resulted in increased rates of directional gamma-prime coarsening during elevated temperature creep exposure.

  8. Influence of cobalt, tantalum, and tungsten on the microstructure and mechanical properties of superalloy single crystals

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Ebert, L. J.

    1982-01-01

    The influence of Co, Ta, and W on the microstructure and mechanical properties of nickel base super-alloy single crystals was investigated. A matrix of alloys was based on Mar-M 247 stripped of C, B, Zr, and Hf. The microstructures of the alloys were examined using optical and electron microscopy, phase extraction, X-ray diffraction, and differential thermal analysis. Tensile and creep-rupture tests were performed at 1000 C. An increase in tensile and creep strength resulted when Co was removed from alloys containing high refractory metal contents, but Co effects were negligible for alloys with lower refractory metal levels. In the composition range studied, W was more effective than Ta in increasing the creep resistance. The mechanical properties are discussed in relation to the microstructures of the alloys.

  9. Yielding and deformation behavior of the single crystal superalloy PWA 1480

    NASA Technical Reports Server (NTRS)

    Milligan, Walter W.; Antolovich, Stephen D.

    1987-01-01

    Interrupted tensile tests were conducted to fixed plastic strain levels in 100 ordered single crystals of the nickel based superalloy PWA 1480. Testing was done in the range of 20 to 1093 C, at strain rate of 0.5 and 50 percent/min. The yield strength was constant from 20 to 760 C, above which the strength dropped rapidly and became a strong function of strain rate. The high temperature data were represented very well by an Arrhenius type equation, which resulted in three distinct temperature regimes. The deformation substructures were grouped in the same three regimes, indicating that there was a fundamental relationship between the deformation mechanisms and activation energies. Models of the yielding process were considered, and it was found that no currently available model was fully applicable to this alloy. It was also demonstrated that the initial deformation mechanism (during yielding) was frequently different from that which would be inferred by examining specimens which were tested to failure.

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

    NASA Astrophysics Data System (ADS)

    Basak, Amrita; Acharya, Ranadip; Das, Suman

    2016-08-01

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

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

    NASA Astrophysics Data System (ADS)

    Basak, Amrita; Acharya, Ranadip; Das, Suman

    2016-06-01

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

  12. Growth of shaped single crystals of proteins

    NASA Astrophysics Data System (ADS)

    Moreno, Abel; Rondón, Deyanira; García-Ruiz, Juan Ma.

    1996-09-01

    We present a procedure for obtaining protein single crystals that fill the capillary tubes in which they grow. The implementation was typical of the gel acupuncture method and the four different proteins are used as examples: lysozyme (HEW), thaumatin I, ferritin and insulin. Rod- and prismatic-shaped protein single crystals of these four proteins were grown inside capillary tubes of 0.2, 0.3, 0.5 mm in diameter and, for the case of lysozyme, up to 1.2 mm in diameter. The maximum length measured along the long axes of the rod crystals was 1.6 mm again for lysozyme crystals. It was observed that, once the capillary tube was filled, the crystal continues to grow by diffusion of the precipitating agent throughout the porous network formed by the protein crystal structure. We also discuss the possibility of growing these cylinders of crystalline proteins by the addition of protein solution to the mother liquor through the upper end of the glass capillary while the precipitating agent diffuses through the protein crystal itself. X-ray diffraction patterns confirm the single crystal character of the protein rods.

  13. Single Crystals Grown Under Unconstrained Conditions

    NASA Astrophysics Data System (ADS)

    Sunagawa, Ichiro

    Based on detailed investigations on morphology (evolution and variation in external forms), surface microtopography of crystal faces (spirals and etch figures), internal morphology (growth sectors, growth banding and associated impurity partitioning) and perfection (dislocations and other lattice defects) in single crystals, we can deduce how and by what mechanism the crystal grew and experienced fluctuation in growth parameters through its growth and post-growth history under unconstrained condition. The information is useful not only in finding appropriate way to growing highly perfect and homogeneous single crystals, but also in deciphering letters sent from the depth of the Earth and the Space. It is also useful in discriminating synthetic from natural gemstones. In this chapter, available methods to obtain molecular information are briefly summarized, and actual examples to demonstrate the importance of this type of investigations are selected from both natural minerals (diamond, quartz, hematite, corundum, beryl, phlogopite) and synthetic crystals (SiC, diamond, corundum, beryl).

  14. Fatigue hardening in niobium single crystals.

    NASA Technical Reports Server (NTRS)

    Doner, M.; Diprimio, J. C.; Salkovitz, E. I.

    1973-01-01

    Nb single crystals of various orientations were cyclically deformed in tension-compression under strain control. At low strain amplitudes all crystals oriented for single slip and some oriented for multiple slip showed a two stage hardening. When present, the first stage was characterized with almost no cyclic work hardening. The rate of hardening in the second stage increased with strain amplitude and the amount of secondary slip. In crystals oriented for single slip kink bands developed on their side faces during rapid hardening stage which resulted in considerable amount of asterism in Laue spots. A cyclic stress-strain curve independent of prior history was found to exist which was also independent of crystal orientation. Furthermore, this curve differed only slightly from that of polycrystalline Nb obtained from data in literature.

  15. Development of two rhenium- containing superalloys for single- crystal blade and directionally solidified vane applications in advanced turbine engines

    NASA Astrophysics Data System (ADS)

    Harris, K.; Erickson, G. L.; Sikkenga, S. L.; Brentnall, W. D.; Aurrecoechea, J. M.; Kubarych, K. G.

    1993-08-01

    A team approach involving several turbine engine companies using the concepts of simultaneous engi-neering has been used to successfully develop CMSX-4 ® alloy for turbine blade applications. CMSX-4 al-loy is a second-generation, single-crystal cast nickel-base superalloy containing 3% Re and approximately 70% volume fraction of γ. The high level of balanced properties determined by labora-tory evaluation has been confirmed during field testing of the Solarγ Mars T-14000 industrial gas turbine with CMSX-4 single-crystal (SX) blades in both the coated and bare condition. A similar collaborative ap-proach has resulted in the successful development of CM 186 LCγ alloy for complex, directionally solidi-fied (DS) columnar grain vane segments. CM 186 LC alloy is a second-generation DS columnar grain cast nickel-base superalloy containing 3% Re and approximately 65% volume fraction of γ. Excellent com-ponent producibility and quality is demonstrated. Turbine engine testing is scheduled to commence by the end of 1993.

  16. Effect of tensile mean stress on fatigue behavior of single-crystal and directionally solidified superalloys

    NASA Technical Reports Server (NTRS)

    Kalluri, Sreeramesh; Mcgaw, Michael A.

    1990-01-01

    Two nickel base superalloys, single crystal PWA 1480 and directionally solidified MAR-M 246 + Hf, were studied in view of the potential usage of the former and usage of the latter as blade materials for the turbomachinery of the space shuttle main engine. The baseline zero mean stress (ZMS) fatigue life (FL) behavior of these superalloys was established, and then the effect of tensile mean stress (TMS) on their FL behavior was characterized. At room temperature these superalloys have lower ductilities and higher strengths than most polycrystalline engineering alloys. The cycle stress-strain response was thus nominally elastic in most of the fatigue tests. Therefore, a stress range based FL prediction approach was used to characterize both the ZMS and TMS fatigue data. In the past, several researchers have developed methods to account for the detrimental effect of tensile mean stress on the FL for polycrystalline engineering alloys. However, the applicability of these methods to single crystal and directionally solidified superalloys has not been established. In this study, these methods were applied to characterize the TMS fatigue data of single crystal PWA 1480 and directionally solidified MAR-M 246 + Hf and were found to be unsatisfactory. Therefore, a method of accounting for the TMS effect on FL, that is based on a technique proposed by Heidmann and Manson was developed to characterize the TMS fatigue data of these superalloys. Details of this method and its relationship to the conventionally used mean stress methods in FL prediction are discussed.

  17. Investigation of Advanced Processed Single-Crystal Turbine Blade Alloys

    NASA Technical Reports Server (NTRS)

    Peters, B. J.; Biondo, C. M.; DeLuca, D. P.

    1995-01-01

    This investigation studied the influence of thermal processing and microstructure on the mechanical properties of the single-crystal, nickel-based superalloys PWA 1482 and PWA 1484. The objective of the program was to develop an improved single-crystal turbine blade alloy that is specifically tailored for use in hydrogen fueled rocket engine turbopumps. High-gradient casting, hot isostatic pressing (HIP), and alternate heat treatment (HT) processing parameters were developed to produce pore-free, eutectic-free microstructures with different (gamma)' precipitate morphologies. Test materials were cast in high thermal gradient solidification (greater than 30 C/cm (137 F/in.)) casting furnaces for reduced dendrite arm spacing, improved chemical homogeneity, and reduced interdendritic pore size. The HIP processing was conducted in 40 cm (15.7 in.) diameter production furnaces using a set of parameters selected from a trial matrix study. Metallography was conducted on test samples taken from each respective trial run to characterize the as-HIP microstructure. Post-HIP alternate HT processes were developed for each of the two alloys. The goal of the alternate HT processing was to fully solution the eutectic gamma/(gamma)' phase islands and to develop a series of modified (gamma)' morphologies for subsequent characterization testing. This was accomplished by slow cooling through the (gamma)' solvus at controlled rates to precipitate volume fractions of large (gamma)'. Post-solution alternate HT parameters were established for each alloy providing additional volume fractions of finer precipitates. Screening tests included tensile, high-cycle fatigue (HCF), smooth and notched low-cycle fatigue (LCF), creep, and fatigue crack growth evaluations performed in air and high pressure (34.5 MPa (5 ksi)) hydrogen at room and elevated temperature. Under the most severe embrittling conditions (HCF and smooth and notched LCF in 34.5 MPa (5 ksi) hydrogen at 20 C (68 F), screening test

  18. Characterization of zinc selenide single crystals

    NASA Technical Reports Server (NTRS)

    Gerhardt, Rosario A.

    1996-01-01

    ZnSe single crystals of high quality and low impurity levels are desired for use as substrates in optoelectronic devices. This is especially true when the device requires the formation of homoepitaxial layers. While ZnSe is commercially available, it is at present extremely expensive due to the difficulty of growing single crystal boules with low impurity content and the resultant low yields. Many researchers have found it necessary to heat treat the crystals in liquid Zn in order to remove the impurities, lower the resistivity and activate the photoluminescence at room temperature. The physical vapor transport method (PVT) has been successfully used at MSFC to grow many single crystals of II-VI semiconducting materials including ZnSe. The main goal at NASA has been to try to establish the effect of gravity on the growth parameters. To this effect, crystals have been grown vertically upwards or horizontally. Both (111) and (110) oriented ZnSe crystals have been obtained via unseeded PVT growth. Preliminary characterization of the horizontally grown crystals has revealed that Cu is a major impurity and that the low temperature photoluminescence spectra is dominated by the copper peak. The ratio of the copper peak to the free exciton peak is being used to determine variations in composition throughout the crystal. It was the intent of this project to map the copper composition of various crystals via photoluminescence first, then measure their electrical resistivity and capacitance as a function of frequency before proceeding with a heat treatment designed to remove the copper impurities. However, equipment difficulties with the photoluminescence set up, having to establish a procedure for measuring the electrical properties of the as-grown crystals and time limitations made us re-evaluate the project goals. Vertically grown samples designated as ZnSe-25 were chosen to be measured electrically since they were not expected to show as much variation in their

  19. Effects of substrate crystallographic orientations on crystal growth and microstructure development in laser surface-melted superalloy single crystals. Mathematical modeling of single-crystal growth in a melt pool (Part II)

    SciTech Connect

    Liu Weiping . E-mail: wel2@lehigh.edu; DuPont, J.N.

    2005-03-01

    The mathematical model developed for single-crystalline solidification in laser surface melting (LSM) described in Part I [Acta Mater 2004;52:4833-4847] was used to compute the dendrite growth pattern and velocity distribution in the 3D melt pool for various substrate orientations. LSM experiments with single-crystal nickel-base superalloys were conducted for different orientations to verify the computational results. Results show that the substrate orientation has a predominant effect on crystal growth pattern, and simultaneously influences the magnitude and distribution of dendrite growth velocity in the melt pool. The selected <100> growth variants and the number of the chosen growth variants are dependent on the substrate orientation. The maximum velocity ratio (dendrite growth velocity over the beam velocity, V/V{sub b}) in the melt pool is a function of melt-pool geometrical parameters and the substrate orientation. The largest maximum velocity-ratio among the symmetric orientations is 1.414 for the (001)/[110] and (011)/[011-bar] orientations, while that value for asymmetric orientations is 1.732 for the (011)/[111-bar] orientation. Good agreement was obtained between the predicted and experimentally observed microstructures. The results are discussed with the susceptibility to stray grain formation as a function of substrate orientations and melt-pool geometrical parameters. These findings have some important implications for single-crystal surface processing.

  20. Neutron detection with single crystal organic scintillators

    NASA Astrophysics Data System (ADS)

    Zaitseva, Natalia P.; Newby, Jason; Hamel, Sebastien; Carman, Leslie; Faust, Michelle; Lordi, Vincenzo; Cherepy, Nerine J.; Stoeffl, Wolfgang; Payne, Stephen A.

    2009-08-01

    Detection of high-energy neutrons in the presence of gamma radiation background utilizes pulse-shape discrimination (PSD) phenomena in organics studied previously only with limited number of materials, mostly liquid scintillators and single crystal stilbene. The current paper presents the results obtained with broader varieties of luminescent organic single crystals. The studies involve experimental tools of crystal growth and material characterization in combination with the advanced computer modeling, with the final goal of better understanding the relevance between the nature of the organic materials and their PSD properties. Special consideration is given to the factors that may diminish or even completely obscure the PSD properties in scintillating crystals. Among such factors are molecular and crystallographic structures that determine exchange coupling and exciton mobility in organic materials and the impurity effect discussed on the examples of trans-stilbene, bibenzyl, 9,10- diphenylanthracene and diphenylacetylene.

  1. Neutron detection with single crystal organic scintillators

    SciTech Connect

    Zaitseva, N; Newby, J; Hamel, S; Carman, L; Faust, M; Lordi, V; Cherepy, N; Stoeffl, W; Payne, S

    2009-07-15

    Detection of high-energy neutrons in the presence of gamma radiation background utilizes pulse-shape discrimination (PSD) phenomena in organics studied previously only with limited number of materials, mostly liquid scintillators and single crystal stilbene. The current paper presents the results obtained with broader varieties of luminescent organic single crystals. The studies involve experimental tools of crystal growth and material characterization in combination with the advanced computer modeling, with the final goal of better understanding the relevance between the nature of the organic materials and their PSD properties. Special consideration is given to the factors that may diminish or even completely obscure the PSD properties in scintillating crystals. Among such factors are molecular and crystallographic structures that determine exchange coupling and exciton mobility in organic materials and the impurity effect discussed on the examples of trans-stilbene, bibenzyl, 9,10-diphenylanthracene and diphenylacetylene.

  2. Oxygen Incorporation in Rubrene Single Crystals

    PubMed Central

    Mastrogiovanni, Daniel D. T.; Mayer, Jeff; Wan, Alan S.; Vishnyakov, Aleksey; Neimark, Alexander V.; Podzorov, Vitaly; Feldman, Leonard C.; Garfunkel, Eric

    2014-01-01

    Single crystal rubrene is a model organic electronic material showing high carrier mobility and long exciton lifetime. These properties are detrimentally affected when rubrene is exposed to intense light under ambient conditions for prolonged periods of time, possibly due to oxygen up-take. Using photoelectron, scanning probe and ion-based methods, combined with an isotopic oxygen exposure, we present direct evidence of the light-induced reaction of molecular oxygen with single crystal rubrene. Without a significant exposure to light, there is no reaction of oxygen with rubrene for periods of greater than a year; the crystal's surface (and bulk) morphology and chemical composition remain essentially oxygen-free. Grand canonical Monte Carlo computations show no sorbtion of gases into the bulk of rubrene crystal. A mechanism for photo-induced oxygen inclusion is proposed. PMID:24786311

  3. Remarkable structural diversity and single-crystal-to-single-crystal transformations in sulfone functionalized lanthanide MOFs

    SciTech Connect

    Neofotistou, Eleftheria; Malliakas, Christos D.; Trikalitis, Pantelis N.

    2010-04-13

    We report the formation of novel open framework lanthanide (La, Ce, Pr and Dy) MOFs using the ligand 4,4{prime}-bibenzoic acid-2,2{prime}-sulfone. In the case of Ce and Pr, an unprecedented single-crystal-to-single-crystal transformation at room temperature was discovered.

  4. Single-Crystal-to-Single-Crystal Transformations in One Dimensional Ag-Eu Helical System

    SciTech Connect

    Cai, Yue-Peng; Zhout, Xiu-Xia; Zhout, Zheng-Yuan; Zhu, Shi-Zheng; Thallapally, Praveen K.; Liu, Jun

    2009-07-06

    Single-crystal-to-single-crystal transformation of 1-D 4d-4f coordination polymers have been investigated for the first time. It displays high selectivity for Mg2+ and can be used as magnesium ion-selective luminescent probe. More importantly, we observed the transformation of meso-helical chain to rac-helical chain as a function of temperature.

  5. Single crystals of metal solid solutions

    NASA Technical Reports Server (NTRS)

    Miller, J. F.; Austin, A. E.; Richard, N.; Griesenauer, N. M.; Moak, D. P.; Mehrabian, M. R.; Gelles, S. H.

    1974-01-01

    The following definitions were sought in the research on single crystals of metal solid solutions: (1) the influence of convection and/or gravity present during crystallization on the substructure of a metal solid solution; (2) the influence of a magnetic field applied during crystallization on the substructure of a metal solid solution; and (3) requirements for a space flight experiment to verify the results. Growth conditions for the selected silver-zinc alloy system are described, along with pertinent technical and experimental details of the project.

  6. Graphene single crystals: size and morphology engineering.

    PubMed

    Geng, Dechao; Wang, Huaping; Yu, Gui

    2015-05-13

    Recently developed chemical vapor deposition (CVD) is considered as an effective way to large-area and high-quality graphene preparation due to its ultra-low cost, high controllability, and high scalability. However, CVD-grown graphene film is polycrystalline, and composed of numerous grains separated by grain boundaries, which are detrimental to graphene-based electronics. Intensive investigations have been inspired on the controlled growth of graphene single crystals with the absence of intrinsic defects. As the two most concerned parameters, the size and morphology serve critical roles in affecting properties and understanding the growth mechanism of graphene crystals. Therefore, a precise tuning of the size and morphology will be of great significance in scale-up graphene production and wide applications. Here, recent advances in the synthesis of graphene single crystals on both metals and dielectric substrates by the CVD method are discussed. The review mainly covers the size and morphology engineering of graphene single crystals. Furthermore, recent progress in the growth mechanism and device applications of graphene single crystals are presented. Finally, the opportunities and challenges are discussed. PMID:25809643

  7. Single-Crystal Springs For Accelerometers

    NASA Technical Reports Server (NTRS)

    Vanzandt, Thomas R.; Kaiser, William J.; Kenny, Thomas W.

    1995-01-01

    Thermal noise reduced, enabling use of smaller proof masses. Spring-and-mass accelerometers in which springs made of single-crystal material being developed. In spring-and-mass accelerometer, proof mass attached to one end of spring, and acceleration of object at other end of spring measured in terms of deflection of spring, provided frequency spectrum of acceleration lies well below resonant frequency of spring-and-proof-mass system. Use of single-crystal spring materials instead of such polycrystalline spring materials as ordinary metals makes possible to construct highly sensitive accelerometers (including seismometers) with small proof masses.

  8. Microhardness studies of sulfamic acid single crystal

    NASA Astrophysics Data System (ADS)

    Santhosh Kumar, A.; Joseph, Cyriac; Paulose, Reshmi; R, Rajesh; Joseph, Georgekutty; Louis, Godfrey

    2015-02-01

    Vicker's microhardness study of (100), (010) and (001) faces of a non-linear optical crystal sulfamic acid have been reported. Single crystals of sulfamic acid have been grown by slow evaporation method. The load dependence of the Vickers microhardness of sulfamic acid crystal were investigated and analyzed from the stand point of various theoretical models. Crystal samples in a, b and c-axes exhibit reverse indentation effect which is best described by Meyer's law, Hays-Kendall's approach and proportional specimen resistance (PSR) models. The negative values of load dependent quantities in Hays-Kendall's approach and PSR model suggest that the origin of indentation size effect is associated with the process of relaxation of indentation stresses.

  9. Corrosion of nickel-base alloys

    SciTech Connect

    Scarberry, R.C.

    1985-01-01

    The volume consists of three tutorial lectures and 18 contributed papers. The three tutorial lectures provide state-of-the-art background on the physical metallurgy of nickel-base alloys as it relates to corrosion. Also featured are the mechanisms and applications of these alloys and an insight into the corrosion testing techniques. The three tutorial lecture papers will help acquaint newcomers to this family of alloys with a thorough overview. The contributed papers are categorized into four major topics: general corrosion, stress corrosion cracking, fatigue and localized corrosion. Each topic is key-noted by one invited lecture followed by several contributed papers. The papers in the general corrosion section are wide ranging and cover the aspects of material selection, development of galvanic series in corrosive environments, corrosion resistance characteristics, hydrogen permeation and hydrogen embrittlement of nickel and some nickel-base alloys.

  10. Nonlinear spectroscopy of C60 single crystal

    NASA Astrophysics Data System (ADS)

    Zamboni, Roberto; Muccini, Michele; Danieli, R.; Taliani, Carlo; Mohn, H.; Muller, W.; ter Meer, Hans-Ulrich

    1994-11-01

    Two-photon excitation measurements of C60 single crystal at 4 K have been performed. The TPE spectrum shows a sharp band at 1.846 eV which is assigned to the C60 lowest forbidden Frenkel singlet exciton of T1g symmetry. This assignment is supported by the analysis of Herzberg-Teller induced photoluminescence.

  11. Role of cobalt in nickel base superalloys

    NASA Technical Reports Server (NTRS)

    Jarrett, R.; Barefoot, J.; Tien, J.; Sanchez, J.

    1982-01-01

    The effect of cobalt or substituting for cobalt on the mechanical properties of nickel-based superalloys is discussed. Waspaloy, UDIMET 700, and NIMONIC 115, which are representative of Ni-Cr-Co-Al-Ti-Mo superalloys having different gamma prime contents which are strengthened by a heavily alloyed matrix, coherent gamma prime precipitates, and carbides at the grain boundaries. Microstructure and in situ and extracted phase STEM micro-analysis were used to evaluate the three alloys.

  12. Infrared investigations of 4-hydroxycyanobenzene single crystals.

    PubMed

    Capria, E; Benevoli, L; Perucchi, A; Fraboni, B; Tessarolo, M; Lupi, Stefano; Fraleoni-Morgera, A

    2013-08-01

    4-Hydroxycyanobenzene (4HCB) single crystals (SCs) and polycrystals (PCs) have been analyzed by means of both unpolarized and linearly polarized (LP) infrared (IR) beams. Most of the signals found at room temperature (298 K) were assigned to well-defined vibrational modes. Using an LP-IR beam and keeping the beam polarization aligned with either the a or the b crystal axis, anisotropic spectra of SCs were also attributed. The differences between the LP and unpolarized spectra of SCs are discussed in view of spatially anisotropic vibronic couplings between the benzenic π electrons and the molecular functional groups (FGs), with reference to the overall lattice arrangement and the polarizability of the FGs. In addition, signals suggesting the low-concentration presence of tautomers within the crystal were detected. LP-IR measurements of SCs in the temperature range between 298 and 120 K are also reported and discussed, with particular reference to the hydrogen-bonding-related functional groups of 4HCB, allowing the assignment of OH bending signals that were otherwise not clearly attributable and the inference of an anisotropic shrinking of the crystals. Overall, the presented results show that LP-IR spectroscopy is a valuable tool for noncontact, nondestructive characterization of organic semiconducting single crystals. PMID:23829587

  13. Single crystal functional oxides on silicon

    PubMed Central

    Bakaul, Saidur Rahman; Serrao, Claudy Rayan; Lee, Michelle; Yeung, Chun Wing; Sarker, Asis; Hsu, Shang-Lin; Yadav, Ajay Kumar; Dedon, Liv; You, Long; Khan, Asif Islam; Clarkson, James David; Hu, Chenming; Ramesh, Ramamoorthy; Salahuddin, Sayeef

    2016-01-01

    Single-crystalline thin films of complex oxides show a rich variety of functional properties such as ferroelectricity, piezoelectricity, ferro and antiferromagnetism and so on that have the potential for completely new electronic applications. Direct synthesis of such oxides on silicon remains challenging because of the fundamental crystal chemistry and mechanical incompatibility of dissimilar interfaces. Here we report integration of thin (down to one unit cell) single crystalline, complex oxide films onto silicon substrates, by epitaxial transfer at room temperature. In a field-effect transistor using a transferred lead zirconate titanate layer as the gate insulator, we demonstrate direct reversible control of the semiconductor channel charge with polarization state. These results represent the realization of long pursued but yet to be demonstrated single-crystal functional oxides on-demand on silicon. PMID:26853112

  14. Single crystal complex oxide on flexible substrate

    NASA Astrophysics Data System (ADS)

    Bakaul, Saidur; Serrao, Claudy; Lee, Oukjae; Salahuddin, Sayeef

    Flexible ferroelectrics are needed for various applications such as biocompatible energy harvesting and flexible memory. In this sector, most of the current research is focused on organic piezoelectric materials which have advantage of flexibility but suffers severely from poor energy conversion and generation efficiency. On the contrary, owing to very high electromechanical coupling factor (representing energy conversion efficiency) complex oxides are the best choices as energy harvesting and transduction elements, especially for transforming mechanical energies into electronic energy. Still their usage in energy harvesting is very limited mainly due to the stringent growth conditions of single crystals, high temperature needed for crystallization and lack of flexibility and stretchability. We have shown that single crystal Pb0.8Zr0.2TiO3 can be epitaxially transferred on flexible plastic substrate. The transferred PZT shows 70 uC/cm2 remnant polarization and dielectric constant over 100 even when it is bent. These results suggest the possibility of single crystal complex oxide devices on flexible platform.

  15. Single-crystal disk drive miniactuators

    NASA Astrophysics Data System (ADS)

    Giovanardi, Marco; McKenney, Kevin B.; Rule, John A.; Yoshikawa, Shoko

    2001-08-01

    As hard disk drive areal densities increase at a compound annual growth rate (CAGR) of 60%, disk drives must position the head over increasingly small areas while moving more rapidly to reach the desired position. This results in an increase in vibration disturbance. To meet this demand, many hard disk drive manufactures have created prototype dual-stage actuators employing piezoelectric ceramics for the second stage. These are an attractive means of obtaining higher-bandwidth control due to the low inertia and size of the actuator element. As the technology improves, the next limiting factor will be the amount of displacement obtainable with traditional piezoceramic elements. Under the AXIS (Advanced Crystal Integrated System) Consortium program funded by DARPA, the application of PZN-PT single crystal piezoceramic as a second stage disk drive actuator was studied, based on the fact that the single crystal material provides larger stroke than its traditional PZT counterparts. The transverse (d31) strain of PZN-PT single crystal was measured to be about two times larger than that of PZT-5H ceramic. Both materials were integrated into a disk drive system and compared as second stage actuators. The methodologies used and the servo control techniques applied are also discussed in the paper.

  16. Tensile and compression testing of single-crystal gamma Ti-55.5Al

    SciTech Connect

    Zupan, M.; LaVan, D.; Hemker, K.J.

    1997-12-31

    Gamma based titanium aluminides are considered to be promising high temperature application alloys because of their exceptional high temperature mechanical properties and good oxidation resistance. Moreover, with a density less than half of current nickel based super alloys, the increased power to weight ratio that can be realized by using titanium aluminides is very attractive to the automotive and aircraft industries. Here the orientation and temperature dependence of the flow strength of {gamma}-TiAl is being measured to promote a fundamental understanding of the deformation mechanisms that are active in this alloy. High quality single crystals of {gamma}-Ti-55.5 Al have been grown using an optical float zone furnace, which allows for crystal seeding and provides a containerless growth environment. These crystals have been oriented using back reflection Laue and TEM and cut into microsample tensile specimens by electric discharge machining. The microsample testing technique developed at Johns Hopkins is being utilized to measure the orientation, temperature and tension/compression dependence of the flow strength of TiAl. An outline of the microsample testing techniques that have been developed for this study and preliminary results follow in this paper.

  17. Experimental Investigation of Orthoenstatite Single Crystal Rheology

    NASA Astrophysics Data System (ADS)

    fraysse, G.; Girard, J.; Holyoke, C. W.; Raterron, P.

    2013-12-01

    The plasticity of enstatite, upper mantle second most abundant mineral, is still poorly constrained, mostly because of its high-temperature (T) transformation into proto- and clino-enstatite at low pressure (P). Mackwell (1991, GRL, 18, 2027) reports a pioneer study of protoenstatite (Pbcn) single-crystal rheology, but the results do not directly apply to the orthorhombic (Pbca) mantle phase. Ohuchi et al. (2011, Contri. Mineral. Petrol , 161, 961) carried out deformation experiments at P=1.3 GPa on oriented orthoenstatite crystals, investigating the activity of [001](100) and [001](010) dislocation slip systems; they report the first rheological laws for orthoenstatite crystals. However, strain and stress were indirectly constrained in their experiments, which questioned whether steady state conditions of deformation were achieved. Also, data reported for [001](100) slip system were obtained after specimens had transformed by twinning into clinoenstatite. We report here new data from deformation experiments carried out at high T and P ranging from 3.5 to 6.2 GPa on natural Fe-bearing enstatite single crystals, using the Deformation-DIA apparatus (D-DIA) that equipped the X17B2 beamline of the NSLS (NY, USA). The applied stress and specimen strain rates were measured in situ by X-ray diffraction and imaging techniques (e.g., Raterron & Merkel, 2009, J. Sync. Rad., 16, 748; Raterron et al., 2013, Rev. Sci. Instr., 84, 043906). Three specimen orientations were tested: i) with the compression direction along [101]c crystallographic direction, which forms a 45° angle with both [100] and [001] axes, to investigate [001](100) slip-system activity; ii) along [011]c direction to investigate [001](010) system activity; iii) and along enstatite [125] axis, to activate both slip systems together. Crystals were deformed two by two, to compare slip system activities, or against enstatite aggregates or orientated olivine crystals of known rheology for comparison. Run products

  18. Successful Surface Treatments for Reducing Instabilities in Advanced Nickel-base Superalloys for Turbine Blades

    NASA Technical Reports Server (NTRS)

    Locci, Ivan E.; MacKay, Rebecca A.; Garg, Anita; Ritzert, Frank J.

    2004-01-01

    An optimized carburization treatment has been developed to mitigate instabilities that form in the microstructures of advanced turbine airfoil materials. Current turbine airfoils consist of a single crystal superalloy base that provides the mechanical performance of the airfoil, a thermal barrier coating (TBC) that reduces the temperature of the base superalloy, and a bondcoat between the superalloy and the TBC, that improves the oxidation and corrosion resistance of the base superalloy and the spallation resistance of the TBC. Advanced nickel-base superalloys containing high levels of refractory metals have been observed to develop an instability called secondary reaction zone (SRZ), which can form beneath diffusion aluminide bondcoats. This instability between the superalloy and the bondcoat has the potential of reducing the mechanical properties of thin-wall turbine airfoils. Controlled gas carburization treatments combined with a prior stress relief heat treatment and adequate surface preparation have been utilized effectively to minimize the formation of SRZ. These additional processing steps are employed before the aluminide bondcoat is deposited and are believed to change the local chemistry and local stresses of the surface of the superalloy. This paper presents the detailed processing steps used to reduce SRZ between platinum aluminide bondcoats and advanced single crystal superalloys.

  19. Surface enrichment and grain boundary segregation of niobium in Inconel 718 single- and poly-crystals

    SciTech Connect

    Pang, X.J.; Dwyer, D.J. . Lab. for Surface Science and Technology); Gao, M.; Valerio, P.; Wei, R.P. . Dept. of Mechanical Engineering and Mechanics)

    1994-08-01

    As a part of a program to study the environmental enhancement of creep crack growth in nickel base alloys, an Inconel 718 (IN718) alloy (100) single crystal was prepared for a planned investigation of the kinetics and mechanisms of reactions with oxygen. During the initial surface characterizations, a strong enrichment of niobium (Nb) within the surface region was observed after heating the surface in ultrahigh vacuum (UHV). The extent of enrichment was wholly unexpected on the basis of existing models and experimental observations. The surface compositions of multiphase systems are also known to be strongly temperature dependent. This temperature dependence will certainly affect chemisorption, dissociation and subsequent reaction of gaseous molecules on freshly exposed (crack) surfaces. In this study, therefore, surface composition of IN718 single-crystal samples as a function of temperature was determined in ultra-high vacuum (UHV). This enrichment suggested that Nb may segregate at grain boundaries of polycrystals during heat treatment, and may play an important role in the subsequent environmental enhancement of crack growth. The segregation of niobium at grain boundaries, therefore, was included as a part of the study.

  20. Effect of tensile mean stress on fatigue behavior of single-crystal and directionally solidified superalloys

    NASA Technical Reports Server (NTRS)

    Kalluri, Sreeramesh; Mcgaw, Michael A.

    1992-01-01

    Two nickel base superalloys, single crystal PWA 1480 and directionally solidified MAR-M 246 + Hf, were studied in view of the potential usage of the former and usage of the latter as blade materials for the turbomachinery of the Space Shuttle main engine. The baseline zero mean stress (ZMS) fatigue life (FL) behavior of these superalloys was established, and then the effect of tensile mean stress (TMS) on their FL behavior was characterized. A stress range based FL prediction approach was used to characterize both the ZMS and TMS fatigue data. In the past, several researchers have developed methods to account for the detrimental effect of tensile mean stress on the FL for polycrystalline engineering alloys. These methods were applied to characterize the TMS fatigue data of single crystal PWA 1480 and directionally solidified MAR-M 246 + Hf and were found to be unsatisfactory. Therefore, a method of accounting for the TMS effect on FL, that is based on a technique proposed by Heidmann and Manson was developed to characterize the TMS fatigue data of these superalloys. Details of this method and its relationship to the conventionally used mean stress methods in FL prediction are discussed.

  1. Lightweight optical mirrors formed in single crystal substrate

    NASA Technical Reports Server (NTRS)

    Bly, Vincent T. (Inventor)

    2006-01-01

    This invention is directed to a process for manufacturing a lightweight mirror from a single crystal material, such as single crystal silicon. As a near perfect single crystal material, single crystal silicon has much lower internal stress than a conventional material. This means much less distortion of the optical surface during the light weighting process. After being ground and polished, a single crystal silicon mirror is light weighted by removing material from the back side using ultrasonic machining. After the light weighting process, the single crystal silicon mirror may be used as-is or further figured by conventional polishing or ion milling, depending on the application and the operating wavelength.

  2. Shock Hugoniot of Single Crystal Copper

    SciTech Connect

    Chau, R; Stolken, J; Asoka-Kumar, P; Kumar, M; Holmes, N C

    2009-08-28

    The shock Hugoniot of single crystal copper is reported for stresses below 66 GPa. Symmetric impact experiments were used to measure the Hugoniots of three different crystal orientations of copper, [100], [110], [111]. The photonic doppler velocimetry (PDV) diagnostic was adapted into a very high precision time of arrival detector for these experiments. The measured Hugoniots along all three crystal directions were nearly identical to the experimental Hugoniot for polycrystalline Cu. The predicted orientation dependence of the Hugoniot from MD calculations was not observed. At the lowest stresses, the sound speed in Cu was extracted from the PDV data. The measured sound speeds are in agreement with values calculated from the elastic constants for Cu.

  3. Growth of Solid Solution Single Crystals

    NASA Technical Reports Server (NTRS)

    Lehoczky, Sandor L.; Szofran, Frank R.; Gillies, Donald C.; Watring, Dale A.

    1999-01-01

    The objective of the study is to establish the effects of processing semiconducting, solid solution, single crystals in a microgravity environment on the metallurgical, compositional, electrical, and optical characteristics of the crystals. The alloy system being investigated is the solid solution semiconductor Hg(1-x)Cd(x)Te, with x-values appropriate for infrared detector applications in the 8 to 14 mm wavelength region. Both melt and Te-solvent growth are being performed. The study consists of an extensive ground-based experimental and theoretical research effort followed by flight experimentation where appropriate. The ground-based portion of the investigation also includes the evaluation of the relative effectiveness of stabilizing techniques, such as applied magnetic fields, for suppressing convective flow during the melt growth of the crystals.

  4. The Creep of Single Crystals of Aluminum

    NASA Technical Reports Server (NTRS)

    Johnson, R D; Shober, F R; Schwope, A D

    1953-01-01

    The creep of single crystals of high-purity aluminum was investigated in the range of temperatures from room temperature to 400 F and at resolved-shear-stress levels of 200, 300, and 400 psi. The tests were designed in an attempt to produce data regarding the relation between the rate of strain and the mechanism of deformation. The creep data are analyzed in terms of shear strain rate and the results are discussed with regard to existing creep theories. Stress-strain curves were determined for the crystals in tinsel and constant-load-rate tests in the same temperature range to supplement the study of plastic deformation by creep with information regarding the part played by crystal orientation, differences in strain markings, and other variables in plastic deformation.

  5. Single-crystal gallium nitride nanotubes

    NASA Astrophysics Data System (ADS)

    Goldberger, Joshua; He, Rongrui; Zhang, Yanfeng; Lee, Sangkwon; Yan, Haoquan; Choi, Heon-Jin; Yang, Peidong

    2003-04-01

    Since the discovery of carbon nanotubes in 1991 (ref. 1), there have been significant research efforts to synthesize nanometre-scale tubular forms of various solids. The formation of tubular nanostructure generally requires a layered or anisotropic crystal structure. There are reports of nanotubes made from silica, alumina, silicon and metals that do not have a layered crystal structure; they are synthesized by using carbon nanotubes and porous membranes as templates, or by thin-film rolling. These nanotubes, however, are either amorphous, polycrystalline or exist only in ultrahigh vacuum. The growth of single-crystal semiconductor hollow nanotubes would be advantageous in potential nanoscale electronics, optoelectronics and biochemical-sensing applications. Here we report an `epitaxial casting' approach for the synthesis of single-crystal GaN nanotubes with inner diameters of 30-200nm and wall thicknesses of 5-50nm. Hexagonal ZnO nanowires were used as templates for the epitaxial overgrowth of thin GaN layers in a chemical vapour deposition system. The ZnO nanowire templates were subsequently removed by thermal reduction and evaporation, resulting in ordered arrays of GaN nanotubes on the substrates. This templating process should be applicable to many other semiconductor systems.

  6. Biomineralization of nanoscale single crystal hydroxyapatite.

    PubMed

    Omokanwaye, Tiffany; Wilson, Otto C; Gugssa, Ayelle; Anderson, Winston

    2015-11-01

    The chemical and physical characteristics of nanocrystalline hydroxyapatite particles which formed during the subcutaneous implantation of crab shell in Sprague-Dawley rats were studied using selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). The initial SAED characterization evidence indicated the presence of an amorphous calcium phosphate phase. The electron dense nanophase particles which formed in the wound healing zone displayed broad diffuse rings which usually indicate a low crystalline order or amorphous phase. High resolution transmission electron microscopy (HRTEM) revealed that these mineralized regions contained discrete single crystal particles less than 5nm in size. Micrographs taken at successively higher magnifications revealed very small nanoparticles with a hexagonal arrangement of ion channels with characteristic spacing of 0.54nm and 0.23nm. This study revealed that single crystal hydroxyapatite nanoparticles consisting of only a few unit cells formed via a biomineralization directed process. PMID:26249568

  7. Crack growth in single-crystal silicon

    NASA Technical Reports Server (NTRS)

    Chen, C. P.; Leipold, M. H.

    1986-01-01

    Crack growth in single-crystal silicon at room temperature in air was evaluated by double torsion (DT) load-relaxation method and monitored by acoustic emission (AE) technique. Both DT and AE methods indicated lack of subcritical crack growth in silicon. At the critical stress intensity factor, the crack front was found to be jumping several times in a 'mirror' region and then followed by fast crack growth in a 'hackle' region. Hackle marks were found to be associated with plastic deformation at the tip of the fast moving crack. No dislocation etch pits were found in the 'mirror' region, in which crack growth may result from interatomic bonds broken at the crack tip under stress without any plastic deformation. Acoustic emission appears to be spontaneously generated from both interatomic bonds broken and dislocation generation at the moving crack tip during the crack growth in single-crystal silicon.

  8. Loop polymer brushes from polymer single crystals

    NASA Astrophysics Data System (ADS)

    Zhou, Tian; Li, Christopher

    2014-03-01

    Loop polymer brushes represent a category of polymer brushes with both chain ends being tethered to a surface or interface with sufficiently high density. Due to this morphological difference, loop brushes exhibit distinct properties compared with traditional polymer brushes with single chain end being tethered. In our study, α, ω-functionalized polycaprolactone (PCL) single crystals were prepared as templates for polymer brush synthesis. By carefully controlling crystallization condition and immobilization, looped polymer brushes were successfully prepared. Comprehensive studies on the morphology and physical properties of these polymer brushes were carried out using Atomic Force Microscopy and FTIR. Advantages of using this method include exclusive loop morphology, high grafting density, controlled tethering sites and tunable loop size.

  9. Macrodeformation Twins in Single-Crystal Aluminum.

    PubMed

    Zhao, F; Wang, L; Fan, D; Bie, B X; Zhou, X M; Suo, T; Li, Y L; Chen, M W; Liu, C L; Qi, M L; Zhu, M H; Luo, S N

    2016-02-19

    Deformation twinning in pure aluminum has been considered to be a unique property of nanostructured aluminum. A lingering mystery is whether deformation twinning occurs in coarse-grained or single-crystal aluminum at scales beyond nanotwins. Here, we present the first experimental demonstration of macrodeformation twins in single-crystal aluminum formed under an ultrahigh strain rate (∼10^{6}  s^{-1}) and large shear strain (200%) via dynamic equal channel angular pressing. Large-scale molecular dynamics simulations suggest that the frustration of subsonic dislocation motion leads to transonic deformation twinning. Deformation twinning is rooted in the rate dependences of dislocation motion and twinning, which are coupled, complementary processes during severe plastic deformation under ultrahigh strain rates. PMID:26943543

  10. Optimizing Scale Adhesion on Single Crystal Superalloys

    NASA Technical Reports Server (NTRS)

    Smialek, James L.; Pint, Bruce A.

    2000-01-01

    To improve scale adhesion, single crystal superalloys have been desulfurized to levels below 1 ppmw by hydrogen annealing. A transition to fully adherent behavior has been shown to occur at a sulfur level of about 0.2 ppmw, as demonstrated for PWA 1480, PWA 1484, and Rene N5 single crystal superalloys in 1100-1150 C cyclic oxidation tests up to 2000 h. Small additions of yttrium (15 ppmw) also have been effective in producing adhesion for sulfur contents of about 5 ppmw. Thus the critical Y/S ratio required for adhesion was on the order of 3-to-1 by weight (1-to-1 atomic), in agreement with values estimated from solubility products for yttrium sulfides. While hydrogen annealing greatly improved an undoped alloy, yielding <= 0.01 ppmw S, it also produced benefits for Y-doped alloys without measurably reducing the sulfur content.

  11. Crack Growth in Single-Crystal Silicon

    NASA Technical Reports Server (NTRS)

    Chen, C. P.; Leipold, M. H.

    1986-01-01

    Report describes experiments on crack growth in single-crystal silicon at room temperature in air. Crack growth in (111) cleavage plane of wafers, 50 by 100 by 0.76 mm in dimension, cut from Czochralski singlecrystal silicon studied by double-torsion load-relaxation method and by acoustic-emission measurements. Scanning electron microscopy and X-ray topography also employed. Results aid in design and fabrication of silicon photovoltaic and microelectronic devices.

  12. Ionic diffusion in single crystals of vermiculite

    SciTech Connect

    Maraqah, H.R.

    1993-01-01

    Novel guest-host compounds, based on single crystal vermiculite, were synthesized by diffusive techniques through a new hydrogen vermiculite. Single crystals were chosen because of the ease of characterization. An investigation of the ion transport properties of these single crystals was done to determine the mechanism of conductivity including the predominant charge carrier. Measurements of the ionic conductivity using impedance spectroscopy and X-ray lattice parameters of the ion-exchanged samples strongly suggest that the native cations and not protons are the major current carriers. Single crystals of hydrogen vermiculite were synthesized at room temperature by ion exchange from sodium-vermiculite using 1 molar acetic acid for a one week. Subsequent ion exchange with other cations was found to be much enhanced. Thus transition metals were exchanged in about a week in contrast to the need of several months using previous methods. The ionic conductivity of hydrogen vermiculite was measured and shown to be much lower than that of many other monovalent cations in the same host lattice. Its enthalpy of motion is also much lower. These marked differences suggest that protonic species do not play a significant role in charge transport in these layered materials. These materials were characterized by x-ray powder diffraction, thermogravimetric analysis and acid-base titration. Hydrogen-vermiculite was found to react with organic bases, like methylamine, ethylamine, n-butylamine, n-hexylamine, n-octylamine, n-decylamine, aniline, acrylamide, methacrylaminde, urea, 1,10phenanthroline, and 1,1phenanthroline ferrous sulfate complex, to undergo ion exchange with metal cations like sodium, zinc, copper(II) ions and polymerization reactions could be performed in the galleries of the structure like pyrrole and aniline. Its behavior was compared with that of powdered montmorillonite.

  13. An improved single crystal adsorption calorimeter

    NASA Astrophysics Data System (ADS)

    Stuck, A.; Wartnaby, C. E.; Yeo, Y. Y.; Stuckless, J. T.; Al-Sarraf, N.; King, D. A.

    1996-04-01

    Significant improvements to the single crystal adsorption calorimeter (SCAC) of Borroni-Bird and King are described. The calorimeter comprises a pulsed molecular beam source, an ultrathin single crystal and an infrared detector. It is calibrated using a chopped laser beam, and the amount of gas adsorbed or reacted per pulse is measured using the King and Wells reflection detector technique. Refinements in the molecular beam system, the optical calibration system, flux calibration system and sticking probability measurement technique have been made. The calorimeter response is accurately linear over a useful energy range; the detection limit is estimated as 10 kJ mol -1; and the accuracy in heats of adsorption for heats above ˜ 80 kJ mol -1 is estimated as ˜ 6%. Comparisons of calorimetric heats with isosteric heats and with desorption energies obtained for reversible systems, such as CO on Ni and Pt single crystal surfaces, generally yield good agreement and give support to the estimate for the absolute accuracy of the instrument.

  14. Single crystal diffraction by synchrotron radiation

    SciTech Connect

    Kvick, A.

    1988-01-01

    The tunability and access to short wavelengths in combination with high intensity and the low divergence of the x-ray radiation produced by synchrotron storage rings opens up new and challenging fields for single crystal diffraction. These areas include microcrystal diffraction, studies of time-dependent phenomena, element selective diffraction, studies of materials under extreme conditions, solution of the crystallographic phase problem either by the use of the wavelength dependency of the anomalous scattering or by direct experimental determination of the phases. Single crystal diffraction from proteins and macromolecules using photographic film as a detection medium has already reached considerable maturity, but high-precision data collections using diffractometers at storage rings are still not routine because of the severe requirements for beam stability over extended periods of time. Development work at institutions such as the National Synchrotron Light Source, The Photon Factory, SSRL, CHESS, Hasylab and Daresbury, however, suggest that synchrotron single-crystal diffraction will become an essential part of the research at the synchrotron storage rings in the near future. 9 refs., 2 figs.

  15. Anisotropy of sapphire single crystal sputtering

    SciTech Connect

    Minnebaev, K. F.; Tolpin, K. A.; Yurasova, V. E.

    2015-08-15

    We have studied the spatial distribution of particles sputtered from the base (0001) plane of a sapphire single crystal with trigonal crystalline lattice (α-Al{sub 2}O{sub 3}) that can be considered a superposition of two hexagonal close packed (hcp) structures–the ideal sublattice of oxygen and a somewhat deformed sublattice of aluminum. It is established that the particles sputtered from the base plane of sapphire are predominantly deposited along the sides of an irregular hexagon with spots at its vertices. The patterns of spots have been also studied for sputtering of particles from the (0001) face of a zinc single crystal with the hcp lattice. The spots of sputtered Zn atoms are arranged at the vertices of concentric equilateral hexagons. In both cases, the observed anisotropy of sputtering is related to focused collisions (direct and assisted focusing) and the channeling process. The chemical composition of spots has been determined in various regions of sputtered sapphire deposition. The results are discussed in comparison to analogous earlier data for secondary ion emission from an α-Al{sub 2}O{sub 3} single crystal.

  16. Single crystal cylinder transducers for sonar applications

    NASA Astrophysics Data System (ADS)

    Robinson, Harold; Stevens, Gerald; Buffman, Martin; Powers, James

    2005-04-01

    A segmented cylinder transducer constructed of single crystal lead magnesium niobate-lead titanate (PMN-PT) has been under development at NUWC and EDO Corporation for several years. The purpose of this development was to provide an extremely compact, high power broadband source. By virtue of their extraordinary material properties, ferroelectric single crystals are the ideal transduction material for developing such compact broadband systems. This presentation shall review the evolution of the transducer design as well as present the results of a successful in-water test conducted at NUWC in October of 2003. It shall be shown that design changes intended to eliminate spurious modes limiting the transducer bandwidth first observed in 2002 were successful, resulting in a transducer with a clean frequency response and an effective coupling factor of 0.85. The measured transducer admittance was in nearly exact agreement with theoretical predictions. The NUWC in-water tests demonstrated that the single crystal cylinder achieved an admittance bandwidth (based on the Stansfield criterion) of over 100%, while the tuned power factor was 0.8 or more over 2.5 octaves of frequency. Additionally, the transducer produced 12 dB higher source levels than a similarly sized PZT transducer. [Work sponsored by DARPA.

  17. Charge transport in single crystal organic semiconductors

    NASA Astrophysics Data System (ADS)

    Xie, Wei

    Organic electronics have engendered substantial interest in printable, flexible and large-area applications thanks to their low fabrication cost per unit area, chemical versatility and solution processability. Nevertheless, fundamental understanding of device physics and charge transport in organic semiconductors lag somewhat behind, partially due to ubiquitous defects and impurities in technologically useful organic thin films, formed either by vacuum deposition or solution process. In this context, single-crystalline organic semiconductors, or organic single crystals, have therefore provided the ideal system for transport studies. Organic single crystals are characterized by their high chemical purity and outstanding structural perfection, leading to significantly improved electrical properties compared with their thin-film counterparts. Importantly, the surfaces of the crystals are molecularly flat, an ideal condition for building field-effect transistors (FETs). Progress in organic single crystal FETs (SC-FETs) is tremendous during the past decade. Large mobilities ~ 1 - 10 cm2V-1s-1 have been achieved in several crystals, allowing a wide range of electrical, optical, mechanical, structural, and theoretical studies. Several challenges still remain, however, which are the motivation of this thesis. The first challenge is to delineate the crystal structure/electrical property relationship for development of high-performance organic semiconductors. This thesis demonstrates a full spectrum of studies spanning from chemical synthesis, single crystal structure determination, quantum-chemical calculation, SC-OFET fabrication, electrical measurement, photoelectron spectroscopy characterization and extensive device optimization in a series of new rubrene derivatives, motivated by the fact that rubrene is a benchmark semiconductor with record hole mobility ~ 20 cm2V-1s-1. With successful preservation of beneficial pi-stacking structures, these rubrene derivatives form

  18. A nanoporous two-dimensional polymer by single-crystal-to-single-crystal photopolymerization

    NASA Astrophysics Data System (ADS)

    Kissel, Patrick; Murray, Daniel J.; Wulftange, William J.; Catalano, Vincent J.; King, Benjamin T.

    2014-09-01

    In contrast to the wide number and variety of available synthetic routes to conventional linear polymers, the synthesis of two-dimensional polymers and unambiguous proof of their structure remains a challenge. Two-dimensional polymers—single-layered polymers that form a tiling network in exactly two dimensions—have potential for use in nanoporous membranes and other applications. Here, we report the preparation of a fluorinated hydrocarbon two-dimensional polymer that can be exfoliated into single sheets, and its characterization by high-resolution single-crystal X-ray diffraction analysis. The procedure involves three steps: preorganization in a lamellar crystal of a rigid monomer bearing three photoreactive arms, photopolymerization of the crystalline monomers by [4 + 4] cycloaddition, and isolation of individual two-dimensional polymer sheets. This polymer is a molecularly thin (~1 nm) material that combines precisely defined monodisperse pores of ~9 Å with a high pore density of 3.3 × 1013 pores cm-2. Atomic-resolution single-crystal X-ray structures of the monomer, an intermediate dimer and the final crystalline two-dimensional polymer were obtained and prove the single-crystal-to-single-crystal nature and molecular precision of the two-dimensional photopolymerization.

  19. Single crystal x-ray diffraction: optical and micro hardness studies on chalcone derivative single crystal

    NASA Astrophysics Data System (ADS)

    Crasta, Vincent; Ravindrachary, V.; Bhajantri, R. F.; Naveen, S.; Shridar, M. A.; Shashidhara Prasad, J.

    2005-08-01

    1-(4-methylphenyl)-3-(4- N, N dimethyl amino phenyl)-2-propen-1-one, a chalcone derivative nonlinear optical material has been synthesized by standard method. FT-IR and NMR spectral studies have been performed to confirm the molecular structure of the synthesized compound. The single crystals up to a dimension of 13 x 9 x 3 mm3 were grown by slow evaporation method. The grown crystals were transparent in the entire visible region and absorbs in the UV-region. The refractive index has been measured using a He-Ne laser. The grown crystals have been subjected to single crystal X-ray diffraction studies to determine the crystal structure and hence the cell parameters of the crystal. From this study it is found that this compound crystallizes in orthorhombic system with a space group P212121 and corresponding lattice parameters are, a = 7.3610(13) Å, b = 11.651(2) Å, c = 17.6490(17) Å. The Kurtz powder second harmonic generation test shows that the compound is a potential candidate for Photonic application. The micro hardness test on these crystals were carried out and the load dependence hardness was observed

  20. Shear mode properties of single crystal ferroelectrics

    NASA Astrophysics Data System (ADS)

    McLaughlin, E. A.; Robinson, H. C.

    2003-10-01

    Single crystal ferroelectrics or piezocrystals were recently introduced into the electroactive materials community. The 33-mode electromechanical coupling factor of piezocrystals is typically greater than 0.90, which is significantly larger than typical values for piezoelectric ceramics (0.62-0.74). For sonar projector applications this large k33 has been responsible for more than doubling the bandwidth of active sonar arrays over what is currently achievable with ceramics. Last year a crystal grower produced a cut of lead magnesium niobate-lead titanate (PMN-PT) single crystal with piezoelectric shear coefficient values of 7000 pm/V and shear coupling factors of 0.97. (For PZT5H, d15 is 730 pm/V.) This piezocrystal d15 coefficient implies significantly improved sensitivity and signal-to-noise ratio for accelerometers and hydrophones, while the high coupling promises bandwidth increases greater than those realized in 33-mode projectors using piezocrystals. This research studies the shear-mode behavior of PMN-PT piezocrystals for use in sensors and projectors. By measuring the response of the materials to high and low level electrical bias and excitation fields, frequency, and temperature, the materials' effective material properties as a function of these operational variables were determined. [Work sponsored by ONR and NUWC ILIR.

  1. Shock Compression of Ammonium Perchlorate Single Crystals

    NASA Astrophysics Data System (ADS)

    Gupta, Y. M.; Yuan, Gang; Feng, Ruqiang

    1997-07-01

    The shock response of ammonium perchlorate (AP) single crystals has been examined for uniaxial strain compression along the [210] and [001] directions. Quartz gauge and VISAR measurements have provided the wave profiles at the impact surface and after propagation through thin samples (1-3 mm thickness) for peak stresses ranging between 10 and 65 kbar. A two wave structure due to elastic-plastic deformation was observed for both orientations. The measured HEL values for the [210] and [001] orientations were about 4.3 and 3.5 kbar, respectively. Data for the two orientations reveal small stress relaxation effects and small differences due to crystal orientation effects. We have chosen to fit both sets of results with a simple elastic-perfectly plastic model used for isotropic materials. Reasonable agreement between the calculations and experimental results was obtained. Over the stress range examined to date, no evidence of chemical decomposition was observed for the time durations in our experiments.

  2. Welding and brazing of nickel and nickel-base alloys

    NASA Technical Reports Server (NTRS)

    Mortland, J. E.; Evans, R. M.; Monroe, R. E.

    1972-01-01

    The joining of four types of nickel-base materials is described: (1) high-nickel, nonheat-treatable alloys, (2) solid-solution-hardening nickel-base alloys, (3) precipitation-hardening nickel-base alloys, and (4) dispersion-hardening nickel-base alloys. The high-nickel and solid-solution-hardening alloys are widely used in chemical containers and piping. These materials have excellent resistance to corrosion and oxidation, and retain useful strength at elevated temperatures. The precipitation-hardening alloys have good properties at elevated temperature. They are important in many aerospace applications. Dispersion-hardening nickel also is used for elevated-temperature service.

  3. Oxygen binding by single crystals of hemoglobin.

    PubMed

    Rivetti, C; Mozzarelli, A; Rossi, G L; Henry, E R; Eaton, W A

    1993-03-23

    Reversible oxygen binding curves for single crystals of hemoglobin in the T quaternary structure have been measured using microspectrophotometry. Saturations were determined from complete visible spectra measured with light linearly polarized parallel to the a and c crystal axes. Striking differences were observed between the binding properties of hemoglobin in the crystal and those of hemoglobin in solution. Oxygen binding to the crystal is effectively noncooperative, the Bohr effect is absent, and there is no effect of chloride ion. Also, the oxygen affinity is lower than that of the T quaternary structure in solution. The absence of the Bohr effect supports Perutz's hypothesis on the key role of the salt bridges, which are known from X-ray crystallography to remain intact upon oxygenation. The low affinity and absence of the Bohr effect can be explained by a generalization of the MWC-PSK model (Monod, Wyman, & Changeux, 1965; Perutz, 1970; Szabo & Karplus, 1972) in which both high- and low-affinity tertiary conformations, with broken and unbroken salt bridges, respectively, are populated in the T quaternary structure. Because the alpha and beta hemes make different projections onto the two crystal axes, separate binding curves for the alpha and beta subunits could be calculated from the two measured binding curves. The approximately 5-fold difference between the oxygen affinities of the alpha and beta subunits is much smaller than that predicted from the crystallographic study of Dodson, Liddington, and co-workers, which suggested that oxygen binds only to the alpha hemes.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:8457555

  4. Direct Shear of Olivine Single Crystals

    NASA Astrophysics Data System (ADS)

    Tielke, Jacob; Zimmerman, Mark; Kohlstedt, David

    2016-04-01

    Knowledge of the strength of individual dislocation slip systems in olivine is fundamental to understanding the flow behavior and the development of lattice-preferred orientation in olivine-rich rocks. The most direct measurements of the strengths of individual slip systems are from triaxial compression experiments on olivine single crystals. However, such experiments only allow for determination of flow laws for two of the four dominate slip systems in olivine. In order to measure the strengths of the (001)[100] and (100)[001] slip systems independently, we performed deformation experiments on single crystals of San Carlos olivine in a direct shear geometry. Experiments were carried out at temperatures of 1000° to 1300°C, a confining pressure of 300 MPa, shear stresses of 60 to 334 MPa, and resultant shear strain rates of 7.4 x 10‑6 to 6.7 x 10‑4 s‑1. At high-temperature (≥1200°C) and low-stress (≤200 MPa) conditions, the strain rate of crystals oriented for direct shear on either the (001)[100] or the (100)[001] slip system follows a power law relationship with stress, whereas at lower temperatures and higher stresses, strain rate depends exponentially on stress. The flow laws derived from the mechanical data in this study are consistent with a transition from the operation of a climb-controlled dislocation mechanism during power-law creep to the operation of a glide-controlled dislocation mechanism during exponential creep. In the climb-controlled regime, crystals oriented for shear on the (001)[100] slip system are weaker than crystals orientated for shear on the (100)[001] slip system. In contrast, in the glide-controlled regime the opposite is observed. Extrapolation of flow laws determined for crystals sheared in orientations favorable for slip on these two slip systems to upper mantle conditions reveals that the (001)[100] slip system is weaker at temperatures and stresses that are typical of the asthenospheric mantle, whereas the (100

  5. Chemical vapor deposition of graphene single crystals.

    PubMed

    Yan, Zheng; Peng, Zhiwei; Tour, James M

    2014-04-15

    As a two-dimensional (2D) sp(2)-bonded carbon allotrope, graphene has attracted enormous interest over the past decade due to its unique properties, such as ultrahigh electron mobility, uniform broadband optical absorption and high tensile strength. In the initial research, graphene was isolated from natural graphite, and limited to small sizes and low yields. Recently developed chemical vapor deposition (CVD) techniques have emerged as an important method for the scalable production of large-size and high-quality graphene for various applications. However, CVD-derived graphene is polycrystalline and demonstrates degraded properties induced by grain boundaries. Thus, the next critical step of graphene growth relies on the synthesis of large graphene single crystals. In this Account, we first discuss graphene grain boundaries and their influence on graphene's properties. Mechanical and electrical behaviors of CVD-derived polycrystalline graphene are greatly reduced when compared to that of exfoliated graphene. We then review four representative pathways of pretreating Cu substrates to make millimeter-sized monolayer graphene grains: electrochemical polishing and high-pressure annealing of Cu substrate, adding of additional Cu enclosures, melting and resolidfying Cu substrates, and oxygen-rich Cu substrates. Due to these pretreatments, the nucleation site density on Cu substrates is greatly reduced, resulting in hexagonal-shaped graphene grains that show increased grain domain size and comparable electrical properties as to exfoliated graphene. Also, the properties of graphene can be engineered by its shape, thickness and spatial structure. Thus, we further discuss recently developed methods of making graphene grains with special spatial structures, including snowflakes, six-lobed flowers, pyramids and hexagonal graphene onion rings. The fundamental growth mechanism and practical applications of these well-shaped graphene structures should be interesting topics and

  6. Growth rate study of canavalin single crystals

    NASA Technical Reports Server (NTRS)

    Demattei, R. C.; Feigelson, R. S.

    1989-01-01

    The dependence on supersaturation of the growth rate of single crystals of the protein canavalin is studied. In the supersaturation ranges studied, the rate-limiting step for growth is best described by a screw dislocation mechanism associated with interface attachment kinetics. Using a ln-ln plot, the growth-rate data is found to fit a predictive relationship of the form G = 0.012 x the supersaturation to the 6.66, which, together with the solubility curves, allows the growth rate to be estimated under a variety of conditions.

  7. Conduction mechanism of single-crystal alumina

    NASA Technical Reports Server (NTRS)

    Will, Fritz G.; Delorenzi, Horst G.; Janora, Kevin H.

    1992-01-01

    The fully guarded three-terminal technique was used to perform conductivity measurements on single-crystal alumina at temperatures of 400-1300 C. The conductivity was also determined as a function of time at various temperatures and applied fields. Further, the fractions of the current carried by Al and O ions (ionic transference numbers) were determined from long-term transference experiments in the temperature range 1100-1300 C. A mathematical model of the conduction mechanism is proposed, and model predictions are compared with experimental results.

  8. Fiber laser welding of nickel based superalloy Inconel 625

    NASA Astrophysics Data System (ADS)

    Janicki, Damian M.

    2013-01-01

    The paper describes the application of single mode high power fiber laser (HPFL) for the welding of nickel based superalloy Inconel 625. Butt joints of Inconel 625 sheets 0,8 mm thick were laser welded without an additional material. The influence of laser welding parameters on weld quality and mechanical properties of test joints was studied. The quality and mechanical properties of the joints were determined by means of tensile and bending tests, and micro hardness tests, and also metallographic examinations. The results showed that a proper selection of laser welding parameters provides non-porous, fully-penetrated welds with the aspect ratio up to 2.0. The minimum heat input required to achieve full penetration butt welded joints with no defect was found to be 6 J/mm. The yield strength and ultimate tensile strength of the joints are essentially equivalent to that for the base material.

  9. Thermodynamic forces in single crystals with dislocations

    NASA Astrophysics Data System (ADS)

    Van Goethem, Nicolas

    2014-06-01

    A simple model for the evolution of macroscopic dislocation regions in a single crystal is presented. This model relies on maximal dissipation principle within Kröner's geometric description of the dislocated crystal. Mathematical methods and tools from shape optimization theory provide equilibrium relations at the dislocation front, similarly to previous work achieved on damage modelling (J Comput Phys 33(16):5010-5044, 2011). The deformation state variable is the incompatible strain as related to the dislocation density tensor by a relation involving the Ricci curvature of the crystal underlying elastic metric. The time evolution of the model variables follows from a novel interpretation of the Einstein-Hilbert flow in terms of dislocation microstructure energy. This flow is interpreted as the dissipation of non-conservative dislocations, due to the climb mechanism, modelled by an average effect of mesoscopic dislocations moving normal to their glide planes by adding or removing points defects. The model equations are a fourth-order tensor parabolic equation involving the operator "incompatibility," here appearing as a tensorial counterpart of the scalar Laplacian. This work encompasses and generalizes results previously announced (C R Acad Sci Paris Ser I 349:923-927, 2011), with in addition a series of physical interpretations to give a meaning to the newly introduced concepts.

  10. Fabrication of crystals from single metal atoms

    PubMed Central

    Barry, Nicolas P. E.; Pitto-Barry, Anaïs; Sanchez, Ana M.; Dove, Andrew P.; Procter, Richard J.; Soldevila-Barreda, Joan J.; Kirby, Nigel; Hands-Portman, Ian; Smith, Corinne J.; O’Reilly, Rachel K.; Beanland, Richard; Sadler, Peter J.

    2014-01-01

    Metal nanocrystals offer new concepts for the design of nanodevices with a range of potential applications. Currently the formation of metal nanocrystals cannot be controlled at the level of individual atoms. Here we describe a new general method for the fabrication of multi-heteroatom-doped graphitic matrices decorated with very small, ångström-sized, three-dimensional (3D)-metal crystals of defined size. We irradiate boron-rich precious-metal-encapsulated self-spreading polymer micelles with electrons and produce, in real time, a doped graphitic support on which individual osmium atoms hop and migrate to form 3D-nanocrystals, as small as 15 Å in diameter, within 1 h. Crystal growth can be observed, quantified and controlled in real time. We also synthesize the first examples of mixed ruthenium–osmium 3D-nanocrystals. This technology not only allows the production of ångström-sized homo- and hetero-crystals, but also provides new experimental insight into the dynamics of nanocrystals and pathways for their assembly from single atoms. PMID:24861089

  11. Cutting fluid study for single crystal silicon

    SciTech Connect

    Chargin, D.

    1998-05-05

    An empirical study was conducted to evaluate cutting fluids for Single Point Diamond Turning (SPDT) of single crystal silicon. The pH of distilled waster was adjusted with various additives the examine the effect of pH on cutting operations. Fluids which seemed to promote ductile cutting appeared to increase tool wear as well, an undesirable tradeoff. High Ph sodium hydroxide solutions showed promise for further research, as they yielded the best combination of reduced tool wear and good surface finish in the ductile regime. Negative rake tools were verified to improve the surface finish, but the negative rake tools used in the experiments also showed much higher wear than conventional 0{degree} rake tools. Effects of crystallographic orientation on SPDT, such as star patterns of fracture damage forming near the center of the samples, were observed to decrease with lower feedrates. Silicon chips were observed and photographed, indicative of a ductile materials removal process.

  12. High weldability nickel-base superalloy

    DOEpatents

    Gibson, Robert C.; Korenko, Michael K.

    1980-01-01

    This is a nickel-base superalloy with excellent weldability and high strength. Its composition consists essentially of, by weight percent, 10-20 iron, 57-63 nickel, 7-18 chromium, 4-6 molybdenum, 1-2 niobium, 0.2-0.8 silicon, 0.01-0.05 zirconium, 1.0-2.5 titanium, 1.0-2.5 aluminum, 0.02-0.06 carbon, and 0.002-0.015 boron. The weldability and strength of this alloy give it a variety of applications. The long-time structural stability of this alloy together with its low swelling under nuclear radiation conditions, make it especially suitable for use as a duct material and controlling element cladding for sodium-cooled nuclear reactors.

  13. Growth and surface topography of WSe2 single crystal

    NASA Astrophysics Data System (ADS)

    Dixit, Vijay; Vyas, Chirag; Pataniya, Pratik; Jani, Mihir; Pathak, Vishal; Patel, Abhishek; Pathak, V. M.; Patel, K. D.; Solanki, G. K.

    2016-05-01

    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 WSe2 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 WSe2 crystals. Single crystalline nature of the crystals was confirmed by SAED.

  14. Oscillatory reactions on single crystal surfaces

    NASA Astrophysics Data System (ADS)

    Imbihl, R.

    1993-12-01

    Heterogeneous catalytic reactions exhibit under certain conditions kinetic oscillations which have been investigated both with polycrystalline materials and with single crystal surfaces as catalysts. The present paper reviews single-crystal experiments conducted under isothermal, low pressure conditions ( p < 10 -3 mbar). Two different reaction systems have been investigated: catalytic CO oxidation on various Pt and Pd orientations and catalytic NO reduction on Pt(100) using CO, H 2, or NH 3 as the reducing agent. The different reaction systems exhibit a wide variety of interesting phenomena which are well-known in nonlinear dynamics, for example, such as spatiotemporal pattern formation, the existence of Turing structures and the appearance of deterministic chaos, and chemical turbulence. The mechanistic steps leading to the observed phenomena have been investigated and appropriate mathematical models have been formulated and analyzed using bifurcation theory. The driving force for the rate oscillations has been shown to result from structural changes of the substrate in the case of catalytic CO oxidation on Pt surfaces, subsurface oxygen formation in the case of catalytic CO oxidation on Pd surfaces, and in the chemical reaction network described by a vacancy model in the case of the NO reduction reactions.

  15. Influence of cobalt, tantaum and tungsten on the high temperature mechanical properties of single crystal nickel-base superalloys. Ph.D. Thesis - Case Western Reserve Univ.

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.

    1984-01-01

    For alloys with the baseline refractory metal level of 3 percent Ta and 10 percent W, decreases in Co level from 10 to 0 percent resulted in increased tensile strength and creep resistance. Substitution of W for Ta resulted in decreased creep life at high stresses but improved life at low stresses. Substitution of Ni for Ta caused large reductions in tensile strength and creep resistance, and corresponding increases in ductility. For these alloys with low Ta plus W totals, strength was independent of Co level. The increases in tensile strength with increases in refractory metal content were related to the increases in gamma volume fraction and solid solution hardening. Increases in strength as Co level decreased were considered to be the result of coherency strain hardening from the increased lattice mismatch. Dislocation shear through the gamma-gamma interface is considered to be the rate limiting step in the deformation process.

  16. Growing single crystals in silica gel

    NASA Technical Reports Server (NTRS)

    Rubin, B.

    1970-01-01

    Two types of chemical reactions for crystal growing are discussed. The first is a metathetical reaction to produce calcium tartrate tetrahydrate crystals, the second is a decomplexation reaction to produce cuprous chloride crystals.

  17. Piezoelectric single crystals for ultrasonic transducers in biomedical applications.

    PubMed

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

    2014-10-01

    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

  18. Experimental dynamic metamorphism of mineral single crystals

    USGS Publications Warehouse

    Kirby, S.H.; Stern, L.A.

    1993-01-01

    This paper is a review of some of the rich and varied interactions between non-hydrostatic stress and phase transformations or mineral reactions, drawn mainly from results of experiments done on mineral single crystals in our laboratory or our co-authors. The state of stress and inelastic deformation can enter explicitly into the equilibrium phase relations and kinetics of mineral reactions. Alternatively, phase transformations can have prominent effects on theology and on the nature of inelastic deformation. Our examples represent five types of structural phase changes, each of which is distinguished by particular mechanical effects. In increasing structural complexity, these include: (1) displacive phase transformations involving no bond-breaking, which may produce anomalous brittle behavior. A primary example is the a-?? quartz transition which shows anomalously low fracture strength and tertiary creep behavior near the transition temperature; (2) martensitic-like transformations involving transformation strains dominated by shear deformation. Examples include the orthoenstatite ??? clinoenstatite and w u ??rtzite ??? sphalerite transformations; (3) coherent exsolution or precipitation of a mineral solute from a supersaturated solid-solution, with anisotropy of precipitation and creep rates produced under nonhydrostatic stress. Examples include exsolution of corundum from MgO ?? nAl2O3 spinels and Ca-clinopyroxene from orthopyroxene; (4) order-disorder transformations that are believed to cause anomalous plastic yield strengthening, such as MgO - nAl2O3 spinels; and (5) near-surface devolatilization of hydrous silicate single-crystals that produces a fundamental brittleness thought to be connected with dehydration at microcracks at temperatures well below nominal macroscopic dehydration temperatures. As none of these interactions between single-crystal phase transformations and non-hydrostatic stress is understood in detail, this paper serves as a challenge to

  19. 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.

  20. Submicron diameter single crystal sapphire optical fiber

    SciTech Connect

    Hill, Cary; Homa, Daniel; Liu, Bo; Yu, Zhihao; Wang, Anbo; Pickrell, Gary

    2014-10-02

    In this work, a submicron-diameter single crystal sapphire optical fiber was demonstrated via wet acid etching at elevated temperatures. Etch rates on the order 2.3 µm/hr were achievable with a 3:1 molar ratio sulfuric-phosphoric acid solution maintained at a temperature of 343°C. A sapphire fiber with an approximate diameter of 800 nm was successfully fabricated from a commercially available fiber with an original diameter of 50 µm. The simple and controllable etching technique provides a feasible approach to the fabrication of unique waveguide structures via traditional silica masking techniques. The ability to tailor the geometry of sapphire optical fibers is the first step in achieving optical and sensing performance on par with its fused silica counterpart.

  1. Single-crystal AlN nanonecklaces.

    PubMed

    Wang, Huatao; Xie, Zhipeng; Wang, Yiguang; Yang, Weiyou; Zeng, Qingfeng; Xing, Feng; An, Linan

    2009-01-14

    Distinct single-crystal aluminum nitride nanonecklaces with uniform [1011] faceted beads are synthesized via catalyst-assisted nitriding of Al. The detailed morphology and structure of the nanonecklaces have been characterized. The growth process has been investigated by comparing the products obtained at different synthesis times. The results reveal that the formation of the nanonecklaces is via a process consisting of facet formation and bead unification. The formation of the [1011] facets is due to the presence of a liquid phase that lowers the surface tension of otherwise high-energy [1011] planes. The bead unification is driven by minimizing the energy contributed by surface energy and electrostatic energy. The unique morphology of the nanonecklaces could be useful for studying fundamental physical phenomena and fabricating nanodevices. PMID:19417280

  2. Electrical switching in cadmium boracite single crystals

    NASA Technical Reports Server (NTRS)

    Takahashi, T.; Yamada, O.

    1981-01-01

    Cadmium boracite single crystals at high temperatures ( 300 C) were found to exhibit a reversible electric field-induced transition between a highly insulative and a conductive state. The switching threshold is smaller than a few volts for an electrode spacing of a few tenth of a millimeter corresponding to an electric field of 100 to 1000 V/cm. This is much smaller than the dielectric break-down field for an insulator such as boracite. The insulative state reappears after voltage removal. A pulse technique revealed two different types of switching. Unstable switching occurs when the pulse voltage slightly exceeds the switching threshold and is characterized by a pre-switching delay and also a residual current after voltage pulse removal. A stable type of switching occurs when the voltage becomes sufficiently high. Possible device applications of this switching phenomenon are discussed.

  3. Lattice effects in YVO 3 single crystal

    NASA Astrophysics Data System (ADS)

    Marquina, C.; Sikora, M.; Ibarra, M. R.; Nugroho, A. A.; Palstra, T. T. M.

    2005-04-01

    In this paper we report on the lattice effects in the Mott insulator yttrium orthovanadate (YVO3). Linear thermal expansion and magnetostriction experiments have been performed on a single crystal, in the temperature range from 5 K to room temperature. The YVO3 orders antiferromagnetically at TN=116 K and orbital ordering was reported to appear below TOO=196 K. A first-order structural phase transition takes place at TS=77 K, accompanied by changes in the antiferromagnetic type of ordering as well as in the orbital-ordering type. Our results reveal that the thermal expansion measurement technique is a very powerful tool in order to clearly detect the existence of the above-mentioned transitions. The magnetostriction results point to the stability of the low-temperature-magnetic ground state under such high applied magnetic field.

  4. Low-cobalt single crystal Rene 150

    NASA Technical Reports Server (NTRS)

    Scheuermann, C. M.

    1982-01-01

    The effects of cobalt content on a single crystal version of the advanced, high gamma prime content turbine airfoil alloy Rene 150 were investigated. Cobalt contents under investigation include 12 wt.% (composition level of Rene 150), 6 wt.%, and 0 wt.%. Preliminary test results are presented and compared with the properties of standard DS Rene 150. DTA results indicate that the liquidus goes through a maximum of about 1435 C near 6 wt.% Co. The solidus remains essentially constant at 1390 C with decreasing Co content. The gamma prime solvus appears to go through a minimum of about 1235 C near 6 wt.% Co content. Preliminary as-cast tensile and stress rupture results are presented along with heat treat schedules and future test plans.

  5. Submicron diameter single crystal sapphire optical fiber

    DOE PAGESBeta

    Hill, Cary; Homa, Daniel; Liu, Bo; Yu, Zhihao; Wang, Anbo; Pickrell, Gary

    2014-10-02

    In this work, a submicron-diameter single crystal sapphire optical fiber was demonstrated via wet acid etching at elevated temperatures. Etch rates on the order 2.3 µm/hr were achievable with a 3:1 molar ratio sulfuric-phosphoric acid solution maintained at a temperature of 343°C. A sapphire fiber with an approximate diameter of 800 nm was successfully fabricated from a commercially available fiber with an original diameter of 50 µm. The simple and controllable etching technique provides a feasible approach to the fabrication of unique waveguide structures via traditional silica masking techniques. The ability to tailor the geometry of sapphire optical fibers ismore » the first step in achieving optical and sensing performance on par with its fused silica counterpart.« less

  6. Method of Making Lightweight, Single Crystal Mirror

    NASA Technical Reports Server (NTRS)

    Bly, Vincent T. (Inventor)

    2015-01-01

    A method of making a mirror from a single crystal blank may include fine grinding top and bottom surfaces of the blank to be parallel. The blank may then be heat treated to near its melting temperature. An optical surface may be created on an optical side of the blank. A protector may be bonded to the optical surface. With the protector in place, the blank may be light weighted by grinding a non-optical surface of the blank using computer controlled grinding. The light weighting may include creating a structure having a substantially minimum mass necessary to maintain distortion of the mirror within a preset limit. A damaged layer of the non-optical surface caused by light weighting may be removed with an isotropic etch and/or repaired by heat treatment. If an oxide layer is present, the entire blank may then be etched using, for example, hydrofluoric acid. A reflecting coating may be deposited on the optical surface.

  7. Crystal growth of large size Dy3Al5O12 garnet single crystals

    NASA Astrophysics Data System (ADS)

    Kimura, Hideo; Sakamoto, Masaru; Numazawa, Takenori; Sato, Mitsunori; Maeda, Hiroshi

    1990-01-01

    Crystal growth conditions using the Czochralski technique were examined in order to be able to grow large-size disprosium-aluminum-garnet single crystals; these are useful as a working material in a practical magnetic refrigeration system. Using the best conditions, large-size bubble-free Dy3Al5O12 single crystals 50 mm in diameter were grown from a stoichiometric melt composition using a seed of Y3Al5O12 single crystal.

  8. A simple low-cost single-crystal NMR setup

    NASA Astrophysics Data System (ADS)

    Vinding, Mads S.; Kessler, Tommy O.; Vosegaard, Thomas

    2016-08-01

    A low-cost single-crystal NMR kit is presented along with a web-based post-processing software. The kit consists of a piezo-crystal motor and a goniometer for the crystal, both embedded in a standard wide-bore NMR probe with a 3D printed scaffold. The NMR pulse program controls the angle setting automatically, and the post-processing software incorporates a range of orientation-angle discrepancies present in the kit and other single-crystal setups. Results with a NaNO3 single-crystal show a high degree of reproducibility and excellent agreement with previous findings for the anisotropic quadrupolar interaction.

  9. 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

  10. The stability of lamellar gamma-gamma-prime structures. [nickel-base superalloy

    NASA Technical Reports Server (NTRS)

    Nathal, M. V.; Mackay, R. A.

    1987-01-01

    The stability of stress-annealed gamma/gamma-prime lamellar structures were investigated using three nickel-base single-crystal alloys (the NASAIR 100 and two similar alloys, E and F, containing 5 and 10 wt pct Co, respectively) stress-annealed at 1000 C to form lamellae perpendicular to the applied stress. The rate of the lamellar thickening under various thermal and creep exposures was examined by SEM. For unstressed aging at 1100 C, the lamellar structures of the NASAIR and the E alloys exhibited continuous but slow lamellar coarsening, whereas the lamellae of the alloy F showed pronounced thickening plus spheroidization. Resistance to lamellar thickening was correlated with high magnitudes of lattice mismatch, which promoted a more regular lamellar structure and a finer spacing of misfit dislocations. Specimens which were tension-annealed prior to compressive creep testing exhibited an earlier onset of tertiary creep in comparison with only heat-treated specimens. This was associated with accelerated lamellar coarsening in the stress-annealed specimens.

  11. The characteristics of gamma-prime dislocation pairs in a nickel-base superalloy

    NASA Technical Reports Server (NTRS)

    Gabb, T. P.; Miner, R. V.; Welsch, G.

    1987-01-01

    The gamma-prime dislocation pairs of a single crystal nickel-base superalloy, PWA 1480, after tensile and fatigue loading at 650 C are analyzed. The existence and extent of cube cross slip in octahedral slip, and the nature of gamma-prime dislocation pairs in primary cube slip are investigated. It is observed that the PWA 1480 specimens oriented near (001) and (-3 6 10) line directions deform by octahedral slip and specimens oriented near (-1 1 1) and (-2 3 4) lines deform by primary cube slip. It is determined that the overall dislocation distributions are more homogeneous in low cycle fatigue (LCF) loading than in monotonic tensile loading; however, the gamma-prime dislocation pair characteristics are similar for tensile and LCF test specimens. The data reveal that the gamma-prime dislocation pairs of octahedral slip specimens are near-screw and on the cube cross slip plane and for the cube slip specimens, the dislocation pairs are of various characters and on the primary cube slip plane.

  12. On the Mechanical Behavior of a New Single-Crystal Superalloy for Industrial Gas Turbine Applications

    NASA Astrophysics Data System (ADS)

    Sato, Atsushi; Moverare, Johan J.; Hasselqvist, Magnus; Reed, Roger C.

    2012-07-01

    The mechanical behavior of a new single-crystal nickel-based superalloy for industrial gas turbine (IGT) applications is studied under creep and out-of-phase (OP) thermomechanical fatigue (TMF) conditions. Neutron diffraction methods and thermodynamic modeling are used to quantify the variation of the gamma prime ( γ') strengthening phase around the γ' solvus temperature; these aid the design of primary aging heat treatments to develop either uniform or bimodal microstructures of the γ' phase. Under creep conditions in the temperature range 1023 K to 1123 K (750 °C to 850 °C), with stresses between 235 to 520 MPa, the creep performance is best with a finer and uniform γ' microstructure. On the other hand, the OP TMF performance improves when the γ' precipitate size is larger. Thus, the micromechanical degradation mechanisms occurring during creep and TMF are distinct. During TMF, localized shear banding occurs with the γ' phase penetrated by dislocations; however, during creep, the dislocation activity is restricted to the matrix phase. The factors controlling TMF resistance are rationalized.

  13. Secondary arm coarsening and microsegregation in superalloy PWA-1480 single crystals: Effect of low gravity

    NASA Technical Reports Server (NTRS)

    Vijayakumar, M.; Tewari, S. N.; Lee, J. E.; Curreri, P. A.

    1990-01-01

    Single crystal specimens of nickel base superalloy PWA-1480 were directionally solidified on ground and during low gravity (20 sec) and high gravity (90 sec) parabolic maneuver of KC-135 aircraft. Thermal profiles were measured during solidification by two in-situ thermocouples positioned along the sample length. The samples were quenched during either high or low gravity cycles so as to freeze the structures of the mushy zone developing under different gravity levels. Microsegregation was measured by examining the solutal profiles on several transverse cross-sections across primary dendrites along their length in the quenched mushy zone. Effect of gravity level on secondary arm coarsening kinetics and microsegregation have been investigated. The results indicate that there is no appreciable difference in the microsegregation and coarsening kinetics behavior in the specimens grown under high or low gravity. This suggests that short duration changes in gravity/levels (0.02 to 1.7 g) do not influence convection in the interdendritic region. Examination of the role of natural convection, in the melt near the primary dendrite tips, on secondary arm spacings requires low gravity periods longer than presently available on KC-135. Secondary arm coarsening kinetics show a reasonable fit with the predictions from a simple analytical model proposed by Kirkwood for a binary alloy.

  14. Ultratough CVD single crystal diamond and three dimensional growth thereof

    DOEpatents

    Hemley, Russell J.; Mao, Ho-kwang; Yan, Chih-shiue

    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.

  15. Multifunctional Charge-Transfer Single Crystals through Supramolecular Assembly.

    PubMed

    Xu, Beibei; Luo, Zhipu; Wilson, Andrew J; Chen, Ke; Gao, Wenxiu; Yuan, Guoliang; Chopra, Harsh Deep; Chen, Xing; Willets, Katherine A; Dauter, Zbigniew; Ren, Shenqiang

    2016-07-01

    Centimeter-sized segregated stacking TTF-C60 single crystals are crystallized by a mass-transport approach combined with solvent-vapor evaporation for the first time. The intermolecular charge-transfer interaction in the long-range ordered superstructure enables the crystals to demonstrate external stimuli-controlled multifunctionalities and angle/electrical-potential-dependent luminescence. PMID:27146726

  16. 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.

  17. Microstructure and superconductivity of MgB2 single crystals

    SciTech Connect

    Kim, Kijoon H.P.; Jung, C.U.; Kang, B.W.; Kim, Kyung Hee; Lee, Hyun-Sook; Lee, Sung-Ik; Tamura, N.; Caldwell, W.A.; Patel, J.R.

    2004-07-19

    The hexagonal-disc-shaped MgB2 single crystals were synthesized under the high-pressure conditions. The crystal symmetry, lattice constants as well as the Laue pattern of these single crystals were obtained from X-ray micro-diffraction. A crystallographic mapping showed that the edge and the c-axis of hexagonal-disc shape exactly matched the [1 0 1 bar 0] and [0 0 0 1] directions of the MgB2 phase. This clearly confirmed that above well-shaped single crystals could be excellent samples to study the unsolved direction dependencies of the physical properties.

  18. Double bragg reflections in single crystals and textured polycrystals

    NASA Astrophysics Data System (ADS)

    Skrytnyy, V. I.; Yaltsev, V. N.

    2016-04-01

    Analysis of the detection of the double Bragg reflections (DBR) in single crystals and polycrystals is carried out. Technique of the detection of the double Bragg reflection in single crystals and textured polycrystalline samples using X-ray synchrotron radiation is proposed.

  19. 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)

  20. 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.

  1. Thermally induced single crystal to single crystal transformation leading to polymorphism

    NASA Astrophysics Data System (ADS)

    Saha, Rajat; Biswas, Susobhan; Dey, Sanjoy Kumar; Sen, Arijit; Roy, Madhusudan; Steele, Ian M.; Dey, Kamalendu; Ghosh, Ashutosh; Kumar, Sanjay

    2014-09-01

    The robust complex [La(1,10-phen)2(NO3)3] (1,10-phen = 1,10-phenanthroline) exhibits thermally induced single crystal to single crystal transformation from one polymorphic phase to another. The complex crystallizes in monoclinic C2/c space group with C2 molecular symmetry at 293 K while at 100 K it shows P21/c space group with C1 molecular symmetry. Supramolecular investigation shows that at 100 K the complex forms 2D achiral sheets whereas at 293 K forms two different homochiral 2D sheets. Low temperature DSC analysis indicates that this structural transformation occurs at 246 K and also this transformation is reversible in nature. We have shown that thermally induced coherent movement of ligands changes the molecular symmetry of the complex and leads to polymorphism. Photoluminescence property of complex has been studied in both solid state and in methanolic solution at room temperature. The effect of the presence low-lying LUMO orbital of π-character in the complex is elucidated by theoretical calculation using DFT method.

  2. Directionally solidified eutectic gamma plus beta nickel-base superalloys

    NASA Technical Reports Server (NTRS)

    Jackson, M. R. (Inventor)

    1977-01-01

    A directionally solidified multivariant eutectic gamma + beta nickel-base superalloy casting having improved high temperature strength and oxidation resistance properties is provided. This comprises a two phase eutectic structure containing, on a weight percent basis, 5.0-15.0 tungsten, 8.5-14.5 aluminum, 0.0-35.0 cobalt and the balance being nickel. Embedded within the gamma phase nickel-base matrix are aligned eutectic beta phase (primarily (NiCo)Al reinforcing lamellae.

  3. Microstructure-mechanical property relationships in transient liquid phase bonded nickel-based superalloys and iron-based ODS alloys

    NASA Astrophysics Data System (ADS)

    Aluru, Sreenivasa Charan Rajeev

    The research work presented here discusses the microstructure-mechanical property relationships in wide gap transient liquid phase (TLP) bonds, between the single crystal nickel-base superalloy CMSX-4 and two polycrystalline superalloys, IN 738 and IN 939, using wide-gap style composite interlayers. Fabrication of complicated geometries and successful repair development of gas turbine engine components made of superalloys requires a high performance metallurgical joining technique and a complete understanding of microstructure-mechanical property relationships. A number of joining processes have been investigated, but all of them have significant disadvantages that limit their ability to produce sound joints. TLP bonding has proved to be a successful method and is the most preferred joining method for nickel-based superalloys, with microstructures and compositions of the joint similar to that of the bulk substrates resulting in mechanical properties close to that of the parent metal. The current joining process used two proprietary wide-gap style composite interlayers, Niflex-110 and Niflex-115, consisting of a nickel-based core with boron-rich surfaces, and a conventional rapidly solidified metallic glass foil interlayer BNi-3 was chosen for comparison. When composite interlayers were employed, competition between wetting of the faying surfaces and formation of the eutectic along the grain boundaries was observed to lead to non-bonded regions at the faying surfaces, unless a boron-rich interlayer was employed. Composite interlayers resulted in the suppression of bondline boride formation. With the exception of this competition, adequate wetting of the substrates occurred for all interlayers. Two factors dominated the room temperature mechanical properties of the wide-gap bonds. The first was the extent of gamma-prime formation at the bondline. Results from shear testing and fractography of the bonds indicated ductile shear failure at the bondline. This was due to

  4. Reshock and release response of aluminum single crystal

    NASA Astrophysics Data System (ADS)

    Huang, H.; Asay, J. R.

    2007-03-01

    Reshock and release experiments were performed on single crystal aluminum along three orientations and on polycrystalline 1050 aluminum with 50μm grain size at shock stresses of 13 and 21GPa to investigate the mechanisms for previously observed quasielastic recompression behavior. Particle velocity profiles obtained during reshocking both single crystals and polycrystalline aluminum from initial shock stresses of 13-21GPa show similar quasielastic recompression behavior. Quasielastic release response is also observed in all single crystals, but the magnitude of the effect is crystal orientation dependent, with [111] and [110] exhibiting more ideal elastic-plastic release for unloading from the shocked state than for the [100] orientation and polycrystalline aluminum. The quasielastic response of 1050 aluminum is intermediate to that of the [100] and [111] orientations. Comparison of the wave profiles obtained for both unloading and reloading of single crystals and polycrystalline 1050 aluminum from shocked states suggests that the observed quasielastic response of polycrystalline aluminum results from the averaging response of single crystals for shock propagation along different orientations, and that the response of 1050 aluminum with large grain boundaries is not significantly different from the results obtained on single crystal aluminum. The yield strength of the single crystals and 1050 aluminum is found to increase with shock stress, which is consistent with previous results [H. Huang and I. R. Asay, J. Appl. Phys. 98, 033524 (2005)].

  5. Ferroelectric polarization reversal in single crystals

    NASA Technical Reports Server (NTRS)

    Stadler, Henry L.

    1992-01-01

    Research on the reversal of polarization in ferroelectric crystals is reviewed. Particular attention is given to observation methods for polarization reversal, BaTiO3 polarization reversal, crystal thickness dependence of polarization reversal, and domain wall movement during polarization reversal in TGS.

  6. 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.

  7. Physical properties of superconducting single crystal iron sulfide

    NASA Astrophysics Data System (ADS)

    Rodriguez, Efrain E.; Borg, Christopher K. H.; Zhou, Xiuquan; Paglione, Johnpierre; University of Maryland Collaboration

    Recently, the simple binary tetragonal iron sulfide, FeS, was found to be a superconductor with a Tc = 5 K. We have prepared single crystals of tetragonal iron sulfide through hydrothermal de-intercalation of KxFe2-yS2. The KxFe2-yS2 single crystal precursors were grown by slow cooling of stoichiometric melts of K, Fe and S. The silver, plate-like FeS single crystals were highly crystalline with a superconducting transition temperature (Tc) of 4 K. The high quality of the FeS crystals revealed highly anisotropic nature of the magnetic and electronic properties intrinsic to FeS. The physical properties and thermal stability of single crystal FeS will be discussed in detail.

  8. Method for harvesting single crystals from a peritectic melt

    DOEpatents

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

    1996-01-01

    A method of preparing 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, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals 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 unmelted, allowing the wicking away of the peritectic liquid.

  9. Method for harvesting single crystals from a peritectic melt

    DOEpatents

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

    1996-08-27

    A method of preparing 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, cooling the peritectic mixture to quench directly the mixture on a porous, wettable inert substrate to wick off the peritectic liquid, leaving single crystals 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 unmelted, allowing the wicking away of the peritectic liquid. 2 figs.

  10. Hg-1212 and Hg-1223 single crystals: Synthesis and characterisation

    NASA Astrophysics Data System (ADS)

    Gatt, R.; Olsson, E.; Morawski, A.; Lada, T.; Paszewin, A.; Bryntse, I.; Grishin, A. M.; Eeltsev, Yu.; Berastegui, P.; Johansson, L.-G.

    1997-02-01

    Single crystals of HgBa 2CaCu 2O 6+δ (Hg-1212) and HgBa 2Ca 2Cu 3O 8+δ (Hg-1223) were grown from the melt at an argon pressure of 10 kbar. Electron microscopy, as well as single crystal X-ray diffraction studies show that the crystals are well ordered. The EDS analysis indicates the presence of a minor amount of other cations replacing Hg, Ba and Ca in the structure. Refined fractional coordinates and thermal parameters are given for a crystal of Hg-1223 type. Magnetic and resistive measurements show a Tc of 133 K for the Hg-1223 phase.

  11. 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.

  12. Cloning polymer single crystals through self-seeding

    NASA Astrophysics Data System (ADS)

    Xu, Jianjun; Ma, Yu; Hu, Wenbing; Rehahn, Matthias; Reiter, Günter

    2009-04-01

    In general, when a crystal is molten, all molecules forget about their mutual correlations and long-range order is lost. Thus, a regrown crystal does not inherit any features from an initially present crystal. Such is true for materials exhibiting a well-defined melting point. However, polymer crystallites have a wide range of melting temperatures, enabling paradoxical phenomena such as the coexistence of melting and crystallization. Here, we report a self-seeding technique that enables the generation of arrays of orientation-correlated polymer crystals of uniform size and shape (`clones') with their orientation inherited from an initial single crystal. Moreover, the number density and locations of these cloned crystals can to some extent be predetermined through the thermal history of the starting crystal. We attribute this unique behaviour of polymers to the coexistence of variable fold lengths in metastable crystalline lamellae, typical for ordering of complex chain-like molecules.

  13. Stability of Detached Grown Germanium Single Crystals

    NASA Technical Reports Server (NTRS)

    Schweizer, M.; Volz, M. P.; Cobb, S. D.; Vujisic, L.; Szofran, F. R.; Rose, M. Franklin (Technical Monitor)

    2001-01-01

    Detachment of the melt meniscus from the crucible during semiconductor Bridgman growth experiments has been observed in recent years, especially under microgravity experiments. Under earth conditions, the hydrostatic pressure counteracts the mechanism, whereby it is more difficult to achieve detached Bridgman growth. Attempts to get stable detached growth under terrestrial conditions have been discussed in the literature and have been the subject of recent experiments in our own group. The advantage of crystals grown without wall contact is obvious: In general, they possess a higher crystal quality than conventional Bridgman grown crystals with wall contact. However, due to the interaction of different parameters such as the wetting behavior of the melt with the crucible, and the dependence of the growth angle with the shape of the melt meniscus, the mechanism leading to detachment is very complicated and not completely understood. We have grown several doped and undoped Germanium crystals with the detached Bridgman and the normal Bridgman growth technique. Pyrolytic boron nitride containers were used for all growth experiments. In the detached grown crystals the typical gap thickness between the pBN crucible and the crystal is in the range of 10 to 100 micrometers, which was determined by performing profilometer measurements. Etch pit density measurements were also performed and a comparison between detached and attached grown crystals will be given. An interesting feature was detected on the surface of a detached grown crystal. Strong surface striations with an average axial distance of 0.5 mm were observed around the whole circumference. The maximum fluctuation of the gap thickness is in the range of 5-10 micrometers. These variations of the detached gap along the crystal axis can be explained by a kind of stiction of the melt/crucible interface and thus by a variation of the meniscus shape. This phenomenon leading to the fluctuation of the gap thickness will be

  14. Stability of Detached Grown Germanium Single Crystals

    NASA Technical Reports Server (NTRS)

    Schweizer, M.; Volz, M. P.; Cobb, S. D.; Motakef, S.; Szofran, F. R.; Curreri, Peter A. (Technical Monitor)

    2002-01-01

    Detachment of the melt meniscus from the crucible during semiconductor Bridgman growth experiments has been observed in recent years especially, under microgravity experiments. Under earth conditions, the hydrostatic pressure counteracts the mechanism, whereby it is more difficult to achieve detached Bridgman growth. Attempts to get stable detached growth under terrestrial conditions have been discussed in the literature and have been the subject of recent experiments in our own group. The advantage of crystals grown without wall contact is obvious: In general, they possess a higher crystal quality than conventional Bridgman grown crystals with wall contact. However, due to the interaction of different parameters such as the wetting behavior of the melt with the crucible, and the dependence of the growth angle with the shape of the melt meniscus, the mechanism leading to detachment is very complicated and not completely understood. We have grown several doped and undoped Germanium crystals with the detached Bridgman and the normal Bridgman growth technique. Pyrolytic boron nitride containers were used for all growth experiments. In the detached grown crystals the typical gap thickness between the pBN crucible and the crystal is in the range of 10 to 100 microns, which was determined by performing profilometer measurements. Etch pit density measurements were also performed and a comparison between detached and attached grown crystals will be given. An interesting feature was detected on the surface of a detached grown crystal. Strong surface striations with an average axial distance of 0.5mm were observed around the whole circumference. The maximum fluctuation of the gap thickness is in the range of 5-10 microns. These variations of the detached gap along the crystal axis can be explained by a kind of stiction of the melt/crucible interface and thus by a variation of the meniscus shape. This phenomenon leading to the fluctuation of the gap thickness will be

  15. Fiber laser welding of nickel based superalloy Rene 77

    NASA Astrophysics Data System (ADS)

    Janicki, Damian M.

    2013-01-01

    The study of laser bead-on-plate welding of nickel based superalloy Rene 77 using single mode high power fiber laser has been undertaken to determine the effect of process parameters, such as laser power, welding speed and laser beam defocusing, on the weld geometry and quality. Non-porous and crack-free welds can be achieved for a relatively wide range of fiber laser welding parameters. The welding speed has a major effect on the weld aspect ratio. The laser beam defocusing significantly affects the weld bead geometry, the stability of the keyhole and pore formation. The transition from keyhole mode to conduction mode welding occurs between focal point position +2.0 mm and +4.0 mm. The high porosity was observed at the focal point position of +2.0 mm. The heat input higher than18 J/mm results to hot cracking in the heat affected zone (HAZ). Moreover, it was found that the welds with the weld aspect ratio higher than 1.5 contain cracks, which propagate from the HAZ into the weld metal.

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

    PubMed

    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

    2015-01-01

    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. PMID:26145157

  17. The Growth of Large Single Crystals.

    ERIC Educational Resources Information Center

    Baer, Carl D.

    1990-01-01

    Presented is an experiment which demonstrates principles of experimental design, solubility, and crystal growth and structure. Materials, procedures and results are discussed. Suggestions for adapting this activity to the high school laboratory are provided. (CW)

  18. A Single Crystal Niobium RF Cavity of the TESLA Shape

    SciTech Connect

    W. Singer; X. Singer; P. Kneisel

    2007-09-01

    A fabrication method for single crystal niobium cavities of the TESLA shape was proposed on the basis of metallographic investigations and electron beam welding tests on niobium single crystals. These tests showed that a cavity can be produced without grain boundaries even in the welding area. An appropriate annealing allows the outgassing of hydrogen and stress relaxation of the material without destruction of the single crystal. A prototype single crystal single cell cavity was built. An accelerating gradient of 37.5 MV/m was reached after approximately 110 mu-m of Buffered Chanical Polishing (BCP) and in situ baking at 120°C for 6 hrs with a quality factor exceeding 2x1010 at 1.8 K. The developed fabrication method can be extended to fabrication of multi cell cavities.

  19. A Single Crystal Niobium RF Cavity of the TESLA Shape

    SciTech Connect

    Singer, W.; Singer, X.; Kneisel, P.

    2007-08-09

    A fabrication method for single crystal niobium cavities of the TESLA shape was proposed on the basis of metallographic investigations and electron beam welding tests on niobium single crystals. These tests showed that a cavity can be produced without grain boundaries even in the welding area. An appropriate annealing allows the outgassing of hydrogen and stress relaxation of the material without destruction of the single crystal. A prototype single crystal single cell cavity was build. An accelerating gradient of 37.5 MV/m was reached after approximately 110 {mu}m of Buffered Chemical Polishing (BCP) and in situ baking at 120 deg. C for 6 hrs with a quality factor exceeding 2x1010 at 1.8 K. The developed fabrication method can be extended to fabrication of multi cell cavities.

  20. Single-drop optimization of protein crystallization.

    PubMed

    Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

    2012-08-01

    A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline. PMID:22869140

  1. Single-drop optimization of protein crystallization

    PubMed Central

    Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

    2012-01-01

    A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline. PMID:22869140

  2. Transport in organic single-crystal microbelt for conformal electronics

    NASA Astrophysics Data System (ADS)

    Cui, Nan; Tong, Yanhong; Tang, Qingxin; Liu, Yichun

    2016-03-01

    We showed the advantages of flexible rubrene organic single-crystal microbelts in high-performance devices and circuits towards conformal electronics. The anisotropic transport based on the only one organic microbelt was studied by a "cross-channel" method, and the rubrene microbelt showed the highest mobility up to 26 cm2/V s in the length direction. Based on an individual rubrene microbelt, the organic single-crystal circuit with good adherence on a pearl ball and the gain as high as 18 was realized. These results present great potential for applications of organic single-crystal belts in the next-generation conformal electronics.

  3. UCN Production With a Single Crystal of Ortho-Deuterium

    PubMed Central

    Utsuro, M.; Tanaka, M.; Mishima, K.; Nagai, Y.; Shima, T.; Fukuda, Y.; Kohmoto, T.; Momose, T.; Moriai, A.; Okumura, K.; Yoshino, H.

    2005-01-01

    The present paper reports on the preliminary experimental results concerning a new concept of ultracold neutron production with a single crystal converter of ortho-deuterium lying in the ground rotational state at the low temperature of about 10 K, which should make it possible to utilize a guided cold neutron beam instead of irradiating the converter material in the inside of high radiation fields. The successful observation of the clear Bragg scattering pattern from the single crystal converter and the reasonable results from the first experimental trial of the ultracold neutron production with the single crystal are shown. PMID:27308135

  4. UCN Production With a Single Crystal of Ortho-Deuterium.

    PubMed

    Utsuro, M; Tanaka, M; Mishima, K; Nagai, Y; Shima, T; Fukuda, Y; Kohmoto, T; Momose, T; Moriai, A; Okumura, K; Yoshino, H

    2005-01-01

    The present paper reports on the preliminary experimental results concerning a new concept of ultracold neutron production with a single crystal converter of ortho-deuterium lying in the ground rotational state at the low temperature of about 10 K, which should make it possible to utilize a guided cold neutron beam instead of irradiating the converter material in the inside of high radiation fields. The successful observation of the clear Bragg scattering pattern from the single crystal converter and the reasonable results from the first experimental trial of the ultracold neutron production with the single crystal are shown. PMID:27308135

  5. 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.

  6. Single crystal Processing and magnetic properties of gadolinium nickel

    SciTech Connect

    Shreve, Andrew John

    2012-01-01

    GdNi is a rare earth intermetallic material that exhibits very interesting magnetic properties. Spontaneous magnetostriction occurs in GdNi at T{sub C}, on the order of 8000ppm strain along the c-axis and only until very recently the mechanism causing this giant magnetostriction was not understood. In order to learn more about the electronic and magnetic structure of GdNi, single crystals are required for anisotropic magnetic property measurements. Single crystal processing is quite challenging for GdNi though since the rare-earth transition-metal composition yields a very reactive intermetallic compound. Many crystal growth methods are pursued in this study including crucible free methods, precipitation growths, and specially developed Bridgman crucibles. A plasma-sprayed Gd2O3 W-backed Bridgman crucible was found to be the best means of GdNi single crystal processing. With a source of high-quality single crystals, many magnetization measurements were collected to reveal the magnetic structure of GdNi. Heat capacity and the magnetocaloric effect are also measured on a single crystal sample. The result is a thorough report on high quality single crystal processing and the magnetic properties of GdNi.

  7. Growth and characterization of diammonium copper disulphate hexahydrate single crystal

    SciTech Connect

    Siva Sankari, R.; Perumal, Rajesh Narayana

    2014-03-01

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

  8. Growth and characterization of ammonium acid phthalate single crystals

    NASA Astrophysics Data System (ADS)

    Arunkumar, A.; Ramasamy, P.

    2013-04-01

    Ammonium acid phthalate (AAP) has been synthesized and single crystals were grown by slow evaporation solution growth technique. The unit cell parameters were confirmed by single crystal X-ray diffraction analysis and it belongs to orthorhombic system with the space group of Pcab. The high resolution X-ray diffraction studies revealed the crystalline perfection of the grown crystal. The various functional groups of AAP were identified by FT-IR and Raman spectral analyses. Thermal stability of the grown crystals was studied by TGA/DTA. The optical properties of the grown crystals were analyzed by UV-Vis-NIR and photoluminescence spectral studies. The mechanical property of the grown crystal was studied by Vickers microhardness measurement. The growth features of AAP were analyzed by chemical etching.

  9. A simple low-cost single-crystal NMR setup.

    PubMed

    Vinding, Mads S; Kessler, Tommy O; Vosegaard, Thomas

    2016-08-01

    A low-cost single-crystal NMR kit is presented along with a web-based post-processing software. The kit consists of a piezo-crystal motor and a goniometer for the crystal, both embedded in a standard wide-bore NMR probe with a 3D printed scaffold. The NMR pulse program controls the angle setting automatically, and the post-processing software incorporates a range of orientation-angle discrepancies present in the kit and other single-crystal setups. Results with a NaNO3 single-crystal show a high degree of reproducibility and excellent agreement with previous findings for the anisotropic quadrupolar interaction. PMID:27295612

  10. Growing intermetallic single crystals using in situ decanting

    SciTech Connect

    Petrovic, Cedomir; Canfield, Paul; Mellen, Jonathan

    2012-05-16

    High temperature metallic solution growth is one of the most successful and versatile methods for single crystal growth, and is particularly suited for exploratory synthesis. The method commonly utilizes a centrifuge at room temperature and is very successful for the synthesis of single crystal phases that can be decanted from the liquid below the melting point of the silica ampoule. In this paper, we demonstrate the extension of this method that enables single crystal growth and flux decanting inside the furnace at temperatures above 1200°C. This not only extends the number of available metallic solvents that can be used in exploratory crystal growth but also can be particularly well suited for crystals that have a rather narrow exposed solidification surface in the equilibrium alloy phase diagram.

  11. Twisted Single Crystals of Meta-Aromatic Polyamides

    NASA Astrophysics Data System (ADS)

    Lawrence, D. P.; Martin, D. C.

    1996-03-01

    The morphology of single crystals of the aromatic polyamide poly(metaphenylene isophthalamide) (MPDI or Nomex) was studied by transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The single crystals of MPDI were slowly grown from 0.1 weight percent solution. MPDI forms elongated crystals which aggregate together to form highly regular twisted helical bundles. The repeat periods of the helices typically range from 240 nm to 1000 nm and the bundle diameters vary from 36 nm to 120 nm. The angle between the edge of the crystal and the bundle axis varies from 40 to 65 degrees. The regular twisting evidently arises from a bending moment induced by the triclinic symmetry of the MPDI unit cell and the lamellar geometry of the chain-folded single crystal.

  12. Effect of gamma ray irradiation on sodium borate single crystals

    NASA Astrophysics Data System (ADS)

    Kalidasan, M.; Asokan, K.; Baskar, K.; Dhanasekaran, R.

    2015-12-01

    In this work, the effects of 5 kGy, 10 kGy and 20 kGy doses of gamma ray irradiation on sodium borate, Na2[B4O5(OH)4]·(H2O)8 single crystals have been studied. Initially these crystals were grown by solution growth technique and identified as monoclinic using X-ray diffraction analysis. X-ray rocking curves confirm the formation of crystalline defects due to gamma rays in sodium borate single crystals. The electron paramagnetic resonance spectra have been recorded to identify the radicals created due to gamma ray irradiation in sodium borate single crystals. The thermoluminescence glow curves due to the defects created by gamma rays in this crystal have been observed and their kinetic parameters were calculated using Chen's peak shape method. The optical absorption increases and photoluminescence spectral intensity decreases for 5 kGy and 20 kGy doses gamma ray irradiated crystals compared to pristine and 10 kGy dose irradiated one. The effect of various doses of gamma rays on vibrational modes of the sodium borate single crystals was studied using FT-Raman and ATR-FTIR spectral analysis. The dielectric permittivity, conductance and dielectric loss versus frequency graphs of these crystals have been analyzed to know the effect of gamma ray irradiation on these parameters.

  13. Growth of large single crystals of the orthorhombic paracetamol

    NASA Astrophysics Data System (ADS)

    Mikhailenko, M. A.

    2004-05-01

    A new procedure for the growth of large (cm-range) single crystals of the metastable orthorhombic (s.g. Pcab) polymorph of paracetamol is described. The crystals were grown by very slow cooling of hot water solutions under the conditions, when the multiple nucleation was prevented. The samples were characterized by DSC and X-ray diffraction.

  14. Study of single crystals of metal solid solutions

    NASA Technical Reports Server (NTRS)

    Doty, J. P.; Reising, J. A.

    1973-01-01

    The parameters and requirements for growing single crystals of relatively high melting point metals in a zero gravity environment are studied. The crystal growth of metals such as silver, copper, gold, and alloys with a melting point between 900-1100 C is examined.

  15. Measurement of single crystal surface parameters

    NASA Technical Reports Server (NTRS)

    Swanson, L. W.; Bell, A. E.; Strayer, R. W.

    1972-01-01

    The sticking coefficient and thermal desorption spectra of Cs from the (110) plane of W was investigated. A sticking coefficient of unity for the monolayer region was measured for T 250 K. Several distinct binding states were observed in the thermal desorption spectrum. Work function and electron reflection measurements were made on the (110) and (100) crystal faces of Mo. Both LEED and Auger were used to determine the orientation and cleanliness of the crystal surfaces. The work function values obtained for the (110) and (100) planes of Mo were 4.92 and 4.18 eV respectively.

  16. Growth of single crystals by vapor transport

    NASA Technical Reports Server (NTRS)

    Wiedemeier, H.

    1978-01-01

    The primary objectives of the program were to establish basic vapor transport and crystal growth properties and to determine thermodynamic, kinetic and structural parameters relevant to chemical vapor transport systems for different classes of materials. An important aspect of these studies was the observation of the effects of gravity-caused convection on the mass transport rate and crystal morphology. These objectives were accomplished through extensive vapor transport, thermochemical and structural studies on selected Mn-chalcogenides, II-VI and IV-VI compounds.

  17. High-temperature alloys: Single-crystal performance boost

    NASA Astrophysics Data System (ADS)

    Schütze, Michael

    2016-08-01

    Titanium aluminide alloys are lightweight and have attractive properties for high-temperature applications. A new growth method that enables single-crystal production now boosts their mechanical performance.

  18. 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.

  19. Synthesis, crystal growth and characterization of an organic material: 2-Aminopyridinium succinate succinic acid single crystal.

    PubMed

    Magesh, M; Bhagavannarayana, G; Ramasamy, P

    2015-11-01

    The 2-aminopyridinium succinate succinic acid (2APS) single crystal was synthesized and grown by slow evaporation method. The crystal structure has been confirmed by powder X-ray diffraction as well as single crystal X-ray diffraction analysis. The crystal perfection has been evaluated by high resolution X-ray diffraction (HRXRD). The grown crystal is transparent in the visible and near infrared region. The optical absorption edge was found to be 348 nm. The fluorescence study was carried out by spectrofluorophotometer. The thermal stability of grown crystal was analyzed by thermal gravimetric and differential thermal gravimetric (TG-DTA) analysis. Vicker's hardness study carried out at room temperature shows increased hardness while increasing the load. Laser damage threshold value was determined by Nd:YAG laser operating at 1064 nm. The grown 2APS crystal was characterized by etching studies using water as etchant. PMID:26099828

  20. Single crystal growth and characterization of URu2Si2

    NASA Astrophysics Data System (ADS)

    Haga, Yoshinori; Matsuda, Tatsuma D.; Tateiwa, Naoyuki; Yamamoto, Etsuji; Ōnuki, Yoshichika; Fisk, Zachary

    2014-11-01

    We review recent progress in single crystal growth and study of electronic properties in ?. Czocharalski pulling, using purified uranium metal and subsequent annealing under ultra-high vacuum, is successfully applied to this compound, and it yields the highest residual resistivity ratio. These high-quality single crystals allow us to investigate Fermi surfaces using quantum oscillation and to make detailed transport measurements at low temperature.

  1. 250 W single-crystal fiber Yb:YAG laser.

    PubMed

    Délen, Xavier; Piehler, Stefan; Didierjean, Julien; Aubry, Nicolas; Voss, Andreas; Ahmed, Marwan Abdou; Graf, Thomas; Balembois, Francois; Georges, Patrick

    2012-07-15

    We demonstrate an Yb:YAG single-crystal fiber laser with 251 W output power in continuous-wave and an optical efficiency of 44%. This performance can be explained by the high overlap between pump and signal beams brought by the pump guiding and by the good thermal management provided by the single-crystal fiber geometry. The oscillator performance with a reflectivity of the output coupler as low as 20% also shows high potential for power amplification. PMID:22825171

  2. Inhomogeneities in single crystals of cuprate oxide superconductors

    NASA Technical Reports Server (NTRS)

    Moorjani, K.; Bohandy, J.; Kim, B. F.; Adrian, F. J.

    1991-01-01

    The next stage in the evolution of experimental research on the high temperature superconductors will require high quality single crystals and epitaxially grown crystalline films. However, inhomogeneities and other defects are not uncommon in single crystals of cuprate oxide superconductors, so a corollary requirement will be a reliable method for judging the quality of these materials. The application of magnetically modulated resistance methods in this task is briefly described and illustrated.

  3. Anomalous magneto-resistance in single crystals of silver chalcogenides

    NASA Astrophysics Data System (ADS)

    Zhang, Chenglong; Liu, Haiwen; Hua, Wei; Yuan, Zhunjun; Sun, Junliang; Xie, Xincheng; Jia, Shuang

    2015-03-01

    Silver chalcogenides have been known as quantum materials for over fifteen years but no single crystal was ever studied before. Very recently, we developed a method for growth of single crystals. Our measurements of magneto-resistance (MR) showed strong Shubnikov-de Haas (SdH) oscillations associated with a very low quantum limit. When the field is beyond this limit we observed a negative, longitudinal MR, which is believed as a fingerprint of chiral anomaly in Weyl Fermion systems.

  4. Synthesis and Single-Crystal Growth of Ca

    SciTech Connect

    Nakatsuji, Satoru; Maeno, Yoshiteru

    2001-01-01

    For the study of the quasi-two-dimensional Mott transition system Ca{sub 2-x}Sr{sub x}RuO{sub 4}, we have succeeded in synthesizing polycrystalline samples and also growing single crystals by a floating-zone method. Details of the preparations for the entire solution range are described. The structural, transport, and magnetic properties of both polycrystalline and single-crystal samples are fully in agreement.

  5. Fatigue crack propagation in single-crystal CMSX- 2 at elevated temperature

    NASA Astrophysics Data System (ADS)

    Antolovich, B. F.; Saxena, A.; Antolovich, S. D.

    1993-08-01

    The fatigue crack propagation (FCP) behavior of the nickel-base superalloy CMSX-2 in single-crystal form was investigated. Tests were conducted for two temperatures (25 and 700 °C), two orientations ([001][110] and [001][010]), and in two environments (laboratory air and ultra-high vacuum 10-7 torr). Following FCP testing, the fracture surfaces were examined using scanning electron microscopy (SEM). The FCP rates were found to be relatively independent of the temperature, environment, and orientation when correlated with the conventional mode I stress-intensity factor. Examination of the fracture sur-faces revealed two distinct types of fracture. One type was characterized by 111 fracture surfaces, which were inclined relative to both the loading and crack propagation directions. These features, al-though clearly a result of the fatigue process, resembled cleavage fractures along 111 planes. Such fea-tures were observed at 25 and 700 °C; they were the only features observed for the 25 °C tests. The second type had a macroscopically dull loading appearance, was microscopically rough, and grew normal to the loading axis. These features were observed on the specimens tested at 700 °C (in both air and vacuum) and appeared similar to conventional fatigue fractures. Although in this region the crack plane was mac-roscopically normal to the loading direction, it deviated microscopically to avoid shearing the y ’ precipi-tates. In view of the complex crack growth mechanisms, mixed fracture modes, and lack of any difference in FCP rates, it is hypothesized that the correlation between FCP rates and the stress-intensity parameter is probably coincidental. The implications for life prediction of higher temperature turbine components based on conventional fracture mechanics are significant and should be investigated further.

  6. Optimization of the Homogenization Heat Treatment of Nickel-Based Superalloys Based on Phase-Field Simulations: Numerical Methods and Experimental Validation

    NASA Astrophysics Data System (ADS)

    Rettig, Ralf; Ritter, Nils C.; Müller, Frank; Franke, Martin M.; Singer, Robert F.

    2015-12-01

    A method for predicting the fastest possible homogenization treatment of the as-cast microstructure of nickel-based superalloys is presented and compared with experimental results for the single-crystal superalloy ERBO/1. The computational prediction method is based on phase-field simulations. Experimentally determined compositional fields of the as-cast microstructure from microprobe measurements are being used as input data. The software program MICRESS is employed to account for multicomponent diffusion, dissolution of the eutectic phases, nucleation, and growth of liquid phase (incipient melting). The optimization itself is performed using an iterative algorithm that increases the temperature in such a way that the microstructural state is always very close to the incipient melting limit. Maps are derived allowing describing the dissolution of primary γ/ γ'-islands and the elimination of residual segregation with respect to temperature and time.

  7. Synthesis and characterization of Mo 3Si single crystal

    NASA Astrophysics Data System (ADS)

    Rosales, I.

    2008-08-01

    Mo 3Si single crystals were successfully produced using an optical floating zone furnace. Reoriented specimens were obtained from the original crystal with <1 1 1>, <1 1 0> and <1 0 0> orientations. Cracking behavior of the crystals shows an interesting relation regarding their crystal orientation. Fracture toughness values show small orientation dependence. The hardness test shows that the hard plane is the (1 0 0), and the softest plane was the (1 1 0) and not the (1 1 1) as it was expected.

  8. Optical and photoelectrochemical study of WTe2 single crystals

    NASA Astrophysics Data System (ADS)

    Desai, P. F.; Patel, D. D.; Bhavsar, D. N.; Jani, A. R.

    2013-06-01

    Single crystals of Tungsten Ditelluride (WTe2) having a layered structure grown by chemical vapor transport method using iodine as the transporting agent are studied here. The optical response of these crystals has been obtained by UV-Vis-NIR spectroscopy at room temperature. Results of optical spectra have been analyzed on the basis of three dimensional models. Photoelectrochemical (PEC) characterization of WTe 2 single crystals have been carried out. Photo response measurements were obtained at different intensities of light source to illuminate the photoanode. The effect of intensity in the efficiency of PEC solar cell has been studied. The implications of the results have been discussed.

  9. Growth and characterization of organic single crystal benzyl carbamate

    NASA Astrophysics Data System (ADS)

    Bala Solanki, S. Siva; Perumal, Rajesh Narayana; Suthan, T.; Bhagavannarayana, G.

    2015-10-01

    Benzyl carbamate single crystal is grown by a solution and vertical Bridgman technique for the first time. The cell parameters and morphologies are assessed from single crystal X-ray diffraction analysis. High resolution X-ray diffraction analysis indicates the crystalline perfection of the grown benzyl carbamate crystal. Fourier Transforms Infrared spectroscopy study has been applied to arrive at the different functional groups. Thermo gravimetric analysis and differential scanning calorimetry are used to study its thermal behavior. The microhardness test is carried out and the load dependent hardness is measured.

  10. Vapor crystal growth studies of single crystals of mercuric iodide (3-IML-1)

    NASA Technical Reports Server (NTRS)

    Vandenberg, Lodewijk

    1992-01-01

    A single crystal of mercuric iodide (HgI2) will be grown during the International Microgravity Lab. (IML-1) mission. The crystal growth process takes place by sublimation of HgI2 from an aggregate of purified material, transport of the molecules in the vapor from the source to the crystal, and condensation on the crystal surface. The objectives of the experiment are as follow: to grow a high quality crystal of HgI2 of sufficient size so that its properties can be extensively analyzed; and to study the vapor transport process, specifically the rate of diffusion transport at greatly reduced gravity where convection is minimized.