Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Cobb, Sharon D.; Croell, Arne; Dold, Peter; Kaiser, Natalie; Motakef, Shariar; Schweizer, Marcus; Volz, Martin P.; Vujisic, Ljubomir

2001-01-01

Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in the crystals. In addition to float-zone processing, detached Bridgman growth, although not a completely crucible-free method, is a promising tool to improve crystal quality. It does not suffer from the size limitations of float zoning and the impact of thermocapillary convection on heat and mass transport is expected to be negligible. Detached growth has been observed frequently during (micro)g experiments. Considerable improvements in crystalline quality have been reported for these cases. However, neither a thorough understanding of the process nor a quantitative assessment of the quality of these improvements exists. This project will determine the means to reproducibly grow Pepsi alloys in a detached mode and seeks to compare processing-induced defects in Bridgman, detached-Bridgman, and floating-zone growth configurations in Pepsi crystals (Si less or = 10 at%) up to 20mm in diameter.

Pseudo-transient heat transfer in vertical Bridgman crystal growth of semi-transparent materials

NASA Astrophysics Data System (ADS)

Barvinschi, F.; Nicoara, I.; Santailler, J. L.; Duffar, T.

1998-11-01

The temperature distribution and the solid-liquid interface shape during semi-transparent crystal growth have been studied by modelling a vertical Bridgman technique, using a pseudo-transient approximation in an ideal configuration. The heat transfer equation and the boundary conditions have been solved by the finite-element method. It has been pointed out that the optical absorption coefficients of the liquid and solid phases have a major effect on the thermal field, especially on the shape and location of the crystallization interface.

Investigation of the Crystal Growth of Dielectric Materials by the Bridgman Technique Using Vibrational Control

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.; Zharikov, Evgenii

2002-01-01

The principal goal of this ground-based program, which started on February 1, 1998 and concluded on April 30, 2002, was to investigate the influence of low frequency vibrations on the fluid flow and quality of dielectric oxide crystals grown by the vertical Bridgman method. This experimental program was a collaborative effort between Stanford University and the General Physics Institute of the Russian Academy of Sciences in Moscow, and included a strong emphasis on both physical modeling and the growth of some technologically important materials. Additionally it was carried out initially in collaboration with the theoretical and numerical investigations of A.Fedoseyev and I.Alexander (ongoing in another NASA sponsored program). This latter program involved a study of vibro-convective buoyancy-driven flows in cylindrical configurations with the expectation of being able to use vibrational flows to control buoyancy driven fluid transport to off-set the effect of "g-jitter" during microgravity Bridgman crystal growth. These two programs taken together, were designed to lead to a new parametric control variable which can be used to either suppress or control convection, and thereby heat and mass transport during Bridgman crystal growth. It was expected to be effective in either a terrestrial or space environment.

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

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

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

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

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

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

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

2011-11-15

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

Single Crystal Growth of URu 2Si 2 by the Modified Bridgman Technique

DOE PAGES

Gallagher, Andrew; Nelson, William L.; Chen, Kuan Wen; ...

2016-10-02

We describe a modified Bridgman growth technique to produce single crystals of the strongly correlated electron material URu 2Si 2 and its nonmagnetic analogue ThRu 2Si 2. Bulk thermodynamic and electrical transport measurements show that the properties of crystals produced in this way are comparable to those previously synthesized using the Czochralski or conventional molten metal flux growth techniques. For the specimens reported here, we find residual resistivity ratios RRR = ρ 300K / ρ 0 as large as 116 and 187 for URu 2Si 2 and ThRu 2Si 2, respectively.

The Science of Detached Bridgman Growth and Solutocapillary Convection in Solid Solution Crystals

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Cobb, S. D.; Motakef, S.; Croell, A.; Dold, P.

2001-01-01

Bridgman and Float-zone crystal growth experiments are planned for NASA's First Materials Science Research Rack using the European Space Agency's Materials Science Laboratory with the Low Gradient Furnace (LGF) and Float Zone Furnace with Rotating Magnetic Field (FMF) inserts, respectively. Samples will include germanium and germanium-silicon alloys with up to 10 atomic percent silicon. The Bridgman part of the investigation includes detached growth samples and so there will be a solid-liquid-gas tri-junction in those experiments just as there will be in all float-zone experiments. There are other similarities as well as significant differences between the types of growth that will be discussed. The presentation will call attention to the reasons that experiments in microgravity will provide information unattainable from Earth-based experiments.

On Favorable Thermal Fields for Detached Bridgman Growth

NASA Technical Reports Server (NTRS)

Stelian, Carmen; Volz, Martin P.; Derby, Jeffrey J.

2009-01-01

The thermal fields of two Bridgman-like configurations, representative of real systems used in prior experiments for the detached growth of CdTe and Ge crystals, are studied. These detailed heat transfer computations are performed using the CrysMAS code and expand upon our previous analyses [14] that posited a new mechanism involving the thermal field and meniscus position to explain stable conditions for dewetted Bridgman growth. Computational results indicate that heat transfer conditions that led to successful detached growth in both of these systems are in accordance with our prior assertion, namely that the prevention of crystal reattachment to the crucible wall requires the avoidance of any undercooling of the melt meniscus during the growth run. Significantly, relatively simple process modifications that promote favorable thermal conditions for detached growth may overcome detrimental factors associated with meniscus shape and crucible wetting. Thus, these ideas may be important to advance the practice of detached growth for many materials.

Segregation control in vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Tao, Y.; Kou, S.

1996-11-01

To help the crystal grow at a constant dopant concentration in vertical Bridgman crystal growth, the dopant concentration of the growth melt, i.e. the melt from which the crystal grows, was kept constant. To achieve this, three different methods were used to replenish the growth melt at a controlled rate and suppress dopant diffusion between the growth melt and the replenishing melt. In method one, a replenishing crucible having a long melt passageway was immersed in the growth melt. In method two, a replenishing crucible having an independent feed-rate control mechanism was held above the growth melt. In method three, a submerged diffusion baffle was used to form a long melt passageway between the growth melt and the replenishing melt. NaNO 3 was used as a model material for crystal growth. Single crystals were grown by these three methods with effective segregation control. Method two was applied to InSb and single crystals were also grown with effective segregation control.

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge Si crystal growth experiments are planned to be conducted in the Low 1-x x Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Simulation of solidification in a Bridgman cell

NASA Technical Reports Server (NTRS)

Dakhoul, Y. M.; Farmer, R. C.

1984-01-01

Bridgman-type crystal growth techniques are attractive methods for producing homogeneous, high-quality infrared detector and junction device materials. However, crystal imperfections and interface shapes still must be controlled through modification of the temperature and concentration gradients created during solidification. The objective of this investigation was to study the temperature fields generated by various cell and heatpipe configurations and operating conditions. Continuum's numerical model of the temperature, species concentrations, and velocity fields was used to describe the thermal characteristics of Bridgman cell operation.

One-dimensional thermal modeling of vertical Bridgman-type crystal growth

NASA Technical Reports Server (NTRS)

Jasinski, T.; Naumann, R. J.

1984-01-01

Articles by Naumann (1982) and Jasinski et al. (1983) examined the axial temperature distribution of the charge during vertical Bridgman-type crystal growth. A comparison of their results demonstrates that Naumann's model is applicable for K (ratio of crucible to charge thermal conductivity) equal to or greater than 1 or for small Biot numbers. The Jasinski model provides a correction for larger Biot numbers and is also applicable for small values of K.

Bridgman Growth of Large SrI2:Eu2+ Single Crystals: A High-performance Scintillator for Radiation Detection Applications

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

Boatner, Lynn A; Ramey, Joanne Oxendine; Kolopus, James A

2013-01-01

Single-crystal strontium iodide (SrI2) doped with relatively high levels (e.g., 3 - 6 %) of Eu2+ exhibits characteristics that make this material superior, in a number of respects, to other scintillators that are currently used for radiation detection. Specifically, SrI2:Eu2+ has a light yield that is significantly higher than LaBr3:Ce3+ -a currently employed commercial high-performance scintillator. Additionally, SrI2:Eu2+ is characterized by an energy resolution as high as 2.6% at the 137Cs gamma-ray energy of 662 keV, and there is no radioactive component in SrI2:Eu2+ - unlike LaBr3:Ce3+ that contains 138La. The Ce3+-doped LaBr3 decay time is, however, faster (30 nsec)more » than the 1.2 sec decay time of SrI2:Eu2+. Due to the relatively low melting point of strontium iodide (~515 oC), crystal growth can be carried out in quartz crucibles by the vertical Bridgman technique. Materials-processing and crystal-growth techniques that are specific to the Bridgman growth of europium-doped strontium iodide scintillators are described here. These techniques include the use of a porous quartz frit to physically filter the molten salt from a quartz antechamber into the Bridgman growth crucible and the use of a bent or bulb grain selector design to suppress multiple grain growth. Single crystals of SrI2:Eu2+ scintillators with good optical quality and scintillation characteristics have been grown in sizes up to 5.0 cm in diameter by applying these techniques. Other aspects of the SrI2:Eu2+ crystal-growth methods and of the still unresolved crystal-growth issues are described here.« less

Vertical Bridgman growth of Hg 1-xMn xTe with variational withdrawal rate

NASA Astrophysics Data System (ADS)

Zhi, Gu; Wan-Qi, Jie; Guo-Qiang, Li; Long, Zhang

2004-09-01

Based on the solute redistribution models, Vertical Bridgman growth of Hg1-xMnxTe with variational withdrawal rate is studied. Both theoretical analysis and experimental results show that the axial composition uniformity is improved and the crystal growth rate is also increased at the optimized variational method of withdrawal rate.

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

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

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

2014-04-24

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

Numerical simulation of heat and mass transport during space crystal growth with MEPHISTO

NASA Technical Reports Server (NTRS)

Yao, Minwu; Raman, Raghu; Degroh, Henry C., III

1995-01-01

The MEPHISTO space experiments are collaborative United States and French investigations aimed at understanding the fundamentals of crystal growth. Microgravity experiments were conducted aboard the USMP-1 and -2 missions on STS-52 and 62 in October 1992 and March 1994 respectively. MEPHISTO is a French designed and built Bridgman type furnace which uses the Seebeck technique to monitor the solid/liquid interface temperature and Peltier pulsing to mark the location and shape of the solid/liquid interface. In this paper the Bridgman growth of Sn-Bi and Bi-Sn under terrestrial and microgravity conditions is modeled using the finite element code, FIDAP*. The numerical model considers fully coupled heat and mass transport, fluid motion and solid/liquid phase changes in the crystal growth process. The primary goals of this work are: to provide a quantitative study of the thermal buoyancy-induced convection in the melt for the two flight experiments; to compare the vertical and horizontal growth configurations and systematically evaluate the effects of various gravity levels on the solute segregation. Numerical results of the vertical and horizontal Bridgman growth configurations are presented.

Theoretical analysis of 3D, transient convection and segregation in microgravity Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; de Almeida, Valmor F.; Derby, Jeffrey J.

2000-01-01

We present results from simulations of transient acceleration (g-jitter) in both axial and transverse directions in a simplified prototype of a vertical Bridgman crystal growth system. We also present results on the effects of applying a steady magnetic field in axial or transverse directions to damp the flow. In most cases application of a magnetic field suppresses flow oscillations, but for transverse jitter at intermediate frequencies, flow oscillations grow larger. .

A parametric study of segregation effects during vertical Bridgman crystal growth with an axial magnetic field

NASA Astrophysics Data System (ADS)

Ma, N.; Walker, J. S.

2000-01-01

This paper presents a model for the unsteady transport of a dopant during the vertical Bridgman crystal growth process with a planar crystal-melt interface and with an axial magnetic field, and investigates the effects of varying different process variables on the crystal composition. The convective mass transport due to the buoyant convection in the melt produces nonuniformities in the concentration in both the melt and the crystal. The convective mass transport plays an important role for all magnetic field strengths considered. Diffusive mass transport begins to dominate for a magnetic flux density of 4 T and a fast growth rate, producing crystals which have an axial variation of the radially averaged crystal composition approaching that of the diffusion-controlled limit. Dopant distributions for several different combinations of process parameters are presented.

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science ISS Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processinginduced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croell, A.

2012-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

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

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

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

2014-12-15

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

Radial segregation induced by natural convection and melt/solid interface shape in vertical Bridgman growth

NASA Technical Reports Server (NTRS)

Chang, C. J.; Brown, R. A.

1983-01-01

The roles of natural convection in the melt and the shape of the melt/solid interface on radial dopant segregation are analyzed for a prototype of vertical Bridgman crystal growth system by finite element methods that solve simultaneously for the velocity field in the melt, the shape of the solidification isotherm, and the temperature distribution in both phases. Results are presented for crystal and melt with thermophysical properties similar to those of gallium-doped germanium in Bridgman configurations with melt below (thermally destabilizing) and above (stabilizing) the crystal. Steady axisymmetric flow are classified according to Rayleigh number as either being nearly the growth velocity, having a weak cellular structure or having large amplitude cellular convention. The flows in the two Bridgman configurations are driven by different temperature gradients and are in opposite directions. Finite element calculations for the transport of a dilute dopant by these flow fields reveal radial segregation levels as large as sixty percent of the mean concentration. Segregation is found most severe at an intermediate value of Rayleigh number above which the dopant distribution along the interface levels as the intensity of the flow increases.

Bridgman-Stockbarger growth of SrI2:Eu2+ single crystal

NASA Astrophysics Data System (ADS)

Raja, A.; Daniel, D. Joseph; Ramasamy, P.; Singh, S. G.; Sen, S.; Gadkari, S. C.

2018-05-01

Strontium Iodide (SrI2): Europium Iodide (EuI2) was purified by Zone-refinement process. Europium doped strontium iodide (SrI2:Eu2+) single crystal was grown by modified vertical Bridgman - Stockbarger technique. Photoluminescence (PL) excitation and emission (PLE) spectra were measured for Eu2+ doped SrI2 crystal. The sharp emission was recorded at 432 nm. Scintillation properties of the SrI2:Eu2+ crystal were checked by the gamma ray spectrometer using 137Cs gamma source.

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

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-05-01

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

Passive particle dosimetry. [silver halide crystal growth

NASA Technical Reports Server (NTRS)

Childs, C. B.

1977-01-01

Present methods of dosimetry are reviewed with emphasis on the processes using silver chloride crystals for ionizing particle dosimetry. Differences between the ability of various crystals to record ionizing particle paths are directly related to impurities in the range of a few ppm (parts per million). To understand the roles of these impurities in the process, a method for consistent production of high purity silver chloride, and silver bromide was developed which yields silver halides with detectable impurity content less than 1 ppm. This high purity silver chloride was used in growing crystals with controlled doping. Crystals were grown by both the Czochalski method and the Bridgman method, and the Bridgman grown crystals were used for the experiments discussed. The distribution coefficients of ten divalent cations were determined for the Bridgman crystals. The best dosimeters were made with silver chloride crystals containing 5 to 10 ppm of lead; other impurities tested did not produce proper dosimeters.

Thermal analysis of Bridgman-Stockbarger growth. [mercury cadmium telluride single crystals

NASA Technical Reports Server (NTRS)

Knopf, F. W.

1979-01-01

A thermal analysis of a cylindrical HgCdTe sample in a Bridgman-Stockbarger crystal growth configuration was conducted with emphasis on the thermal profile, interface shape and position, and the thermal gradients at the liquid-solid interface. Alloys of HgTe and CdTe with compositions approximating 20 percent CdTe, 80 percent HgTe were used. This composition results in a bandgap suited for the detection of 10.6 micron CO2 radiation. The sensitivity of the sample thermal characteristics to important growth parameters, such as thermal diffusivities, thermal conductivities, furnace temperature profile, ampoule dimensions, and growth velocity was assessed. Numerical techniques and associated computational models necessary to analyze the heat transfer process within the sample and the Bridgman-Stockbarger boundary conditions were developed. This thermal analysis mode was programmed in FORTRAN V, and is currently operational on the MSFC Univac 1100 system.

Bridgman Growth of Germanium

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Cobb, S. D.; Motakef, S.

1997-01-01

The high-magnetic-field crystal growth facility at the Marshall Space Flight Center will be briefly described. This facility has been used to grow bulk germanium by the Bridgman technique in magnetic fields up to 5 Tesla. The results of investigations of ampoule material on the interface shape and thermal field applied to the melt on stability against convection will be discussed.

The use of magnetic fields in vertical Bridgman/Gradient Freeze-type crystal growth

NASA Astrophysics Data System (ADS)

Pätzold, Olf; Niemietz, Kathrin; Lantzsch, Ronny; Galindo, Vladimir; Grants, Ilmars; Bellmann, Martin; Gerbeth, Gunter

2013-03-01

This paper outlines advanced vertical Bridgman/Gradient Freeze techniques with flow control using magnetic fields developed for the growth of semiconductor crystals. Low-temperature flow modelling, as well as laboratory-scaled crystal growth under the influence of rotating, travelling, and static magnetic fields are presented. Experimental and numerical flow modelling demonstrate the potential of the magnetic fields to establish a well-defined flow for tailoring heat and mass transfer in the melt during growth. The results of the growth experiments are discussed with a focus on the influence of a rotating field on the segregation of dopants, the influence of a travelling field on the temperature field and thermal stresses, and the potential of rotating and static fields for a stabilization of the melt flow.

Prediction of dislocation generation during Bridgman growth of GaAs crystals

NASA Technical Reports Server (NTRS)

Tsai, C. T.; Yao, M. W.; Chait, Arnon

1992-01-01

Dislocation densities are generated in GaAs single crystals due to the excessive thermal stresses induced by temperature variations during growth. A viscoplastic material model for GaAs, which takes into account the movement and multiplication of dislocations in the plastic deformation, is developed according to Haasen's theory. The dislocation density is expressed as an internal state variable in this dynamic viscoplastic model. The deformation process is a nonlinear function of stress, strain rate, dislocation density and temperature. The dislocation density in the GaAs crystal during vertical Bridgman growth is calculated using a nonlinear finite element model. The dislocation multiplication in GaAs crystals for several temperature fields obtained from thermal modeling of both the GTE GaAs experimental data and artificially designed data are investigated.

Prediction of dislocation generation during Bridgman growth of GaAs crystals

NASA Astrophysics Data System (ADS)

Tsai, C. T.; Yao, M. W.; Chait, Arnon

1992-11-01

Dislocation densities are generated in GaAs single crystals due to the excessive thermal stresses induced by temperature variations during growth. A viscoplastic material model for GaAs, which takes into account the movement and multiplication of dislocations in the plastic deformation, is developed according to Haasen's theory. The dislocation density is expressed as an internal state variable in this dynamic viscoplastic model. The deformation process is a nonlinear function of stress, strain rate, dislocation density and temperature. The dislocation density in the GaAs crystal during vertical Bridgman growth is calculated using a nonlinear finite element model. The dislocation multiplication in GaAs crystals for several temperature fields obtained from thermal modeling of both the GTE GaAs experimental data and artificially designed data are investigated.

Influence of Containment on the Growth of Germanium-Silicon in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.; Sorgenfrei, T.

2017-01-01

A series of Ge(sub 1-x)Si(sub x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and 'detached' Bridgman methods and the ground-based float zone technique. 'Detached' or 'dewetted' Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. A meniscus bridges this gap between the top of the crystal and the crucible wall. Theoretical models indicate that an important parameter governing detachment is the pressure differential across this meniscus. An experimental method has been developed to control this pressure differential in microgravity that does not require connection of the ampoule volume to external gases or changes in the temperature profile during growth. Experiments will be conducted with positive, negative or zero pressure differential across the meniscus. Characterization results of ground-based experiments, including etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction will also be described.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

2003-01-01

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Croell, Arne; Dold, Peter; Cobb, Sharon D.; Volz, Martin P.; Motakef, Shariar; Walker, John S.

1999-01-01

It is well established that crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached-Bridgman growth is often cited as a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur quite often during microgravity experiments and considerable improvements of crystal quality have been reported for those cases. However, no thorough understanding of the process or quantitative assessment of the quality improvements exists so far. This project will determine the means to reproducibly grow Ge-Si alloys in the detached mode. Specific objectives include: (1) measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; (2) determination of the mechanism of detached growth including the role of convection; (3) quantitative determination of the differences of defects and impurities among normal Bridgman, detached Bridgman, and floating zone (FZ) growth; (4) investigation of the influence of defined azimuthal or meridional flow due to rotating magnetic fields on the characteristics of detached growth; (5) control time-dependent Marangoni convection in the case of FZ-growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and (6) grow high quality GeSi-single crystals with Si-concentration up to 10 at% and diameters up to 20 mm.

Heat transfer process during the crystallization of benzil grown by the Bridgman-Stockbarger method

NASA Astrophysics Data System (ADS)

Barvinschi, F.; Stanculescu, A.; Stanculescu, F.

2011-02-01

The temperature distribution and solid-liquid interface shape during benzil growth have been studied both experimentally and numerically. The heat transfer equation with appropriate boundary conditions has been solved by modelling a vertical Bridgman-Stockbarger growth configuration. Two models have been developed, namely a global numerical model and a pseudo-transient approximation in an ideal configuration.

Improved radial segregation via the destabilizing vertical Bridgman configuration

NASA Astrophysics Data System (ADS)

Sonda, Paul; Yeckel, Andrew; Daoutidis, Prodromos; Derby, Jeffrey J.

2004-01-01

We employ a computational model to revisit the classic crystal growth experiments conducted by Kim et al. (J. Electrochem. Soc. 119 (1972) 1218) and Müller et al. (J. Crystal Growth 70 (1984) 78), which were among the first to clearly document the effects of flow transitions on segregation. Analysis of the growth of tellerium-doped indium antimonide within a destabilizing vertical Bridgman configuration reveals the existence of multiple states, each of which can be reached by feasible paths of process operation. Transient growth simulations conducted on the different solution branches reveal striking differences in hydrodynamic and segregation behavior. We show that crystals grown in the destabilizing configuration exhibit considerably better radial segregation than those grown in the stabilizing configuration, a result which challenges conventional wisdom and practice.

Numerical Optimization of the Thermal Field in Bridgman Detached Growth

NASA Technical Reports Server (NTRS)

Stelian, C.; Volz, M. P.; Derby, J. J.

2009-01-01

The global modeling of the thermal field in two vertical Bridgman-like crystal growth configurations, has been performed to get optimal thermal conditions for a successful detached growth of Ge and CdTe crystals. These computations are performed using the CrysMAS code and expand upon our previous analysis [1] that propose a new mechanism involving the thermal field and meniscus position to explain stable conditions for dewetted Bridgman growth. The analysis of the vertical Bridgman configuration with two heaters, used by Palosz et al. for the detached growth of Ge, shows, consistent with their results, that the large wetting angle of germanium on boron nitride surfaces was an important factor to promote a successful detached growth. Our computations predict that by initiating growth much higher into the hot zone of the furnace, the thermal conditions will be favorable for continued detachment even for systems that did not exhibit high contact angles. The computations performed for a vertical gradient freeze configuration with three heaters representative of that used for the detached growth of CdTe, show favorable thermal conditions for dewetting during the entirely growth run described. Improved thermal conditions are also predicted for coated silica crucibles when the solid-liquid interface advances higher into the hot zone during the solidification process. The second set of experiments on CdTe growth described elsewhere has shown the reattachment of the crystal to the crucible after few centimeters of dewetted growth. The thermal modeling of this configuration shows a second solidification front appearing at the top of the sample and approaching the middle line across the third heater. In these conditions, the crystal grows detached from the bottom, but will be attached to the crucible in the upper part because of the solidification without gap in this region. The solidification with two interfaces can be avoided when the top of the sample is positioned below the middle position of the third furnace.

Multi-ampoule Bridgman growth of halide scintillator crystals using the self-seeding method

NASA Astrophysics Data System (ADS)

Lindsey, Adam C.; Wu, Yuntao; Zhuravleva, Mariya; Loyd, Matthew; Koschan, Merry; Melcher, Charles L.

2017-07-01

We investigate the multi-ampoule growth at 25 mm diameter of ternary iodide single crystal scintillator KCaI3:Eu using the randomly oriented self-seeded Bridgman method. We compare scintillation performance between cubic inch scale crystals containing small variations of low nominal europium concentrations previously shown to balance light yield with self-absorption in the host crystal. Growth conditions were optimized in the developmental furnace and four 2 in3 KCaI3:Eu crystals were grown simultaneously producing a total of six 25 mm × 25 mm cylinders. Small variations in activator concentration did not result in significant performance differences among the six measured crystals. A range of energy resolutions of 3.5-4.7% at 662 keV was achieved, surpassing that of NaI:Tl crystals commonly used in spectroscopic detection applications. The function and basic design of the multi-ampoule furnace as well as the process of growing single crystals of KCaI3 is included here.

SEMICONDUCTOR MATERIALS: Chemical etching of a GaSb crystal incorporated with Mn grown by the Bridgman method under microgravity conditions

NASA Astrophysics Data System (ADS)

Xiaofeng, Chen; Nuofu, Chen; Jinliang, Wu; Xiulan, Zhang; Chunlin, Chai; Yude, Yu

2009-08-01

A GaSb crystal incorporated with Mn has been grown by the Bridgman method on the Polizon facility onboard the FOTON-M3 spacecraft. Structural defects and growth striations have been successfully revealed by the chemical etching method. By calculating various parameters of the convection, the striation patterns can be explained, and the critical value of the Taylor number, which characterizes the convective condition of the rotating magnetic field induced azimuthal flow, was shown. The stresses generated during crystal growth can be reflected by the observations of etch pit distribution and other structural defects. Suggestions for improving the space experiment to improve the quality of the crystal are given.

A numerical study of steady crystal growth in a vertical Bridgman device

NASA Astrophysics Data System (ADS)

Jalics, Miklos Kalman

Electronics based on semiconductors creates an enormous demand for high quality semiconductor single crystals. The vertical Bridgman device is commonly used for growing single crystals for a variety of materials such as GaAs, InP and HgCdTe. A mathematical model is presented for steady crystal growth under conditions where crystal growth is determined strictly by heat transfer. The ends of the ampoule are chosen far away from the insulation zone to allow for steady growth. A numerical solution is sought for this mathematical model. The equations are transformed into a rectangular geometry and appropriate finite difference techniques are applied on the transformed equations. Newton's method solves the nonlinear problem. To improve efficiency GMRES with preconditioning is used to compute the Newton iterates. The numerical results are used to compare with two current asymptotic theories that assume small Biot numbers. Results indicate that one of the asymptotic theories is accurate for even moderate Biot numbers.

Investigation of Vibrational Control of the Bridgman Crystal Growth Technique

NASA Technical Reports Server (NTRS)

Fedoseyev, Alexandre I.

1998-01-01

The objectives are: Conduct a parametric theoretical and numerical investigation of vibro-convective buoyancy-driven flow in differentially heated cylindrical containers. Investigate buoyant vibro-convective transport regimes in Bridgman-type systems with a focus on the use of vibration to suppress, or control, convection in order to achieve transport control during crystal growth. Assess the feasibility of vibro-convective control as a means of offsetting "g-jitter" effects under microgravity conditions, Exchange information with the experimental group at the General Physics Institute (GPI) of the Russian Academy of Science who are undertaking a complementary experimental program.

Growth of Solid Solution Crystals

NASA Technical Reports Server (NTRS)

Lehoczky, S. L.; Szofran, F. R.; Holland, L. R.

1985-01-01

The major objective of this program is to determine the conditions under which single crystals of solid solutions can be grown from the melt in a Bridgman configuration with a high degree of chemical homogeneity. The central aim is to assess the role of gravity in the growth process and to explore the possible advantages for growth in the absence of gravity. The alloy system being investigated is the solid solution semiconductor with x-values appropriate for infrared detector applications in Hg sub (1-x) Cd sub x Te the 8 to 14 micro m wavelength region. Both melt and Te-solvent growth are being considered. The study consists of an extensive ground-based experimental and theoretical research effort followed by flight experimentation where appropriate. Experimental facilities have been established for the purification, casting, and crystal growth of the alloy system. Facilities have been also established for the metallurgical, compositional, electric and optical characterization of the alloys. Crystals are being grown by the Bridgman-Stockbarger method and are analyzed by various experimental techniques to evaluate the effects of growth conditions on the longitudinal and radial compositional variations and defect densities in the crystals.

Dynamics of melt crystal interface and thermal stresses in rotational Bridgman crystal growth process

NASA Astrophysics Data System (ADS)

Ma, Ronghui; Zhang, Hui; Larson, David J.; Mandal, Krishna C.

2004-05-01

The growth process of potassium bromide (KBr) single crystals in a vertical Bridgman furnace has been studied numerically using an integrated model that combines formulation of global heat transfer and thermal elastic stresses. The global heat transfer sub-model accounts for conduction, convection and interface movement in the multiphase system. Using the elastic stress sub-model, thermal stresses in the growing crystal caused by the non-uniform temperature distribution is predicted. Special attention is directed to the interaction between the crystal and the ampoule. The global temperature distribution in the furnace, the flow pattern in the melt and the interface shapes are presented. We also investigate the effects of the natural convection and rotational forced convection on the shape of the growth fronts. Furthermore, the state of the thermal stresses in the crystal is studied to understand the plastic deformation mechanisms during the cooling process. The influence of the wall contact on thermal stresses is also addressed.

Crystal growth by Bridgman and Czochralski method of the ferromagnetic quantum critical material YbNi4P2

NASA Astrophysics Data System (ADS)

Kliemt, K.; Krellner, C.

2016-09-01

The tetragonal YbNi4P2 is one of the rare examples of compounds that allow the investigation of a ferromagnetic quantum critical point. We report in detail on two different methods which have been used to grow YbNi4P2 single crystals from a self-flux. The first, a modified Bridgman method, using a closed crucible system yields needle-shaped single crystals oriented along the [001]-direction. The second method, the Czochralski growth from a levitating melt, yields large single crystals which can be cut in any desired orientation. With this crucible-free method, samples without flux inclusions and a resistivity ratio at 1.8 K of RR1.8K = 17 have been grown.

Traveling Magnetic Field Applications for Vertical Bridgman Growth: Modeling and Experiment

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin

2004-01-01

Traveling magnetic fields offer a direct control of the metallic melt meridional flow in long cylinders. It induces the Lorentz body force that can counteract with the buoyancy force induced by radial temperature non-uniformity. It can significantly offset a natural convection in the system, or it can even set up the flow in opposite direction, thus affecting the interface shape, the growth rate and macrosegregation. Results of our numerical modeling of the Vertical Bridgman crystal growth of InSb will be discussed. The experimental part of this investigation will address the effect of the applied traveling magnetic fields on the interface shape of InSb crystals. Specifics of the growth apparatus design for this research will be provided in details.

Crystal Growth and Fluid Mechanics Problems in Directional Solidification

NASA Technical Reports Server (NTRS)

Tanveer, Saleh A.; Baker, Gregory R.; Foster, Michael R.

2001-01-01

Our work in directional solidification has been in the following areas: (1) Dynamics of dendrites including rigorous mathematical analysis of the resulting equations; (2) Examination of the near-structurally unstable features of the mathematically related Hele-Shaw dynamics; (3) Numerical studies of steady temperature distribution in a vertical Bridgman device; (4) Numerical study of transient effects in a vertical Bridgman device; (5) Asymptotic treatment of quasi-steady operation of a vertical Bridgman furnace for large Rayleigh numbers and small Biot number in 3D; and (6) Understanding of Mullins-Sererka transition in a Bridgman device with fluid dynamics is accounted for.

Performance testing of a vertical Bridgman furnace using experiments and numerical modeling

NASA Astrophysics Data System (ADS)

Rosch, W. R.; Fripp, A. L.; Debnam, W. J.; Pendergrass, T. K.

1997-04-01

This paper details a portion of the work performed in preparation for the growth of lead tin telluride crystals during a Space Shuttle flight. A coordinated effort of experimental measurements and numerical modeling was completed to determine the optimum growth parameters and the performance of the furnace. This work was done using NASA's Advanced Automated Directional Solidification Furnace, but the procedures used should be equally valid for other vertical Bridgman furnaces.

Superheating Suppresses Structural Disorder in Layered BiI3 Semiconductors Grown by the Bridgman Method

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

Johns, Paul M.; Sulekar, Soumitra; Yeo, Shinyoung

2016-01-01

The susceptibility of layered structures to stacking faults is a problem in some of the more attractive semiconductor materials for ambient-temperature radiation detectors. In the work presented here, Bridgman-grown BiI3 layered single crystals are investigated to understand and eliminate this structural disorder, which reduces radiation detector performance. The use of superheating gradients has been shown to improve crystal quality in non-layered semiconductor crystals; thus the technique was here explored to improve the growth of BiI3. When investigating the homogeneity of non-superheated crystals, highly geometric void defects were found to populate the bulk of the crystals. Applying a superheating gradient tomore » the melt prior to crystal growth improved structural quality and decreased defect density from the order of 4600 voids per cm3 to 300 voids per cm3. Corresponding moderate improvements to electronic properties also resulted from the superheat gradient method of crystal growth. Comparative measurements through infrared microscopy, etch-pit density, x-ray rocking curves, and sheet resistivity readings show that superheat gradients in BiI3 growth led to higher quality crystals.« less

Heat transfer analysis of the Bridgman-Stockbarger configuration for crystal growth. Part 1: Analytical treatment of the axial temperature distribution

NASA Technical Reports Server (NTRS)

Jasinski, T. J.; Rohsenow, W. M.; Witt, A. F.

1982-01-01

All first order effects on the axial temperature distribution in a solidifying charge in a Bridgman-Stockbarger configuration for crystal growth are analyzed on the basis of a one dimensional model whose validity can be verified through comparison with published finite difference ana;uses of two dimensional models. The model presented includes an insulated region between axially aligned heat pipes and considers the effects of charge diameter, charge motion, thickness, and thermal conductivity of a confining crucible, thermal conductivity change at the crystal-melt interface, generation of latent heat at the interface, and finite charge length. Results are primarily given in analytical form and can be used without recourse to computer work for both improve furnace design and optimization of growth conditions in a given thermal configuration.

Influence of Bridgman solidification on microstructures and magnetic behaviors of a non-equiatomic FeCoNiAlSi high-entropy alloy

DOE PAGES

Zuo, Tingting; Yang, Xiao; Liaw, Peter K.; ...

2015-09-07

The non-equiatomic FeCoNiAlSi alloy is prepared by the Bridgman solidification (BS) technique at different withdrawal velocities (V = 30, 100, and 200 μm/s). Various characterization techniques have been used to study the microstructure and crystal orientation. The morphological evolutions accompanying the crystal growth of the alloy prepared at different withdrawal velocities are nearly the same, from equiaxed grains to columnar crystals. The transition of coercivity is closely related to the local microstructure, while the saturation magnetization changes little at different sites. The coercivity can be significantly reduced from the equiaxed grain area to the columnar crystal area when the appliedmore » magnetic field direction is parallel to the crystal growth direction, no matter what is the withdrawal velocity. As a result, the alloy possesses magnetic anisotropy when the applied magnetic field is in different directions.« less

Growth of CdZnTe Crystals the Bridgman Technique with Controlled Overpressures of Cd

NASA Technical Reports Server (NTRS)

Su, Ching-Hu; Lehoczky, S. L.

2008-01-01

Cd(1-x)Zn(x)Te crystals with x = 0.15 and 0.20, were grown in this study by closed-ampoule directional solidification (Bridgman) technique with a controlled Cd overpressure. The growth ampoule was made of quartz with inner diameter from 20 to 40 mm and a tapered length of 2.5 cm at the growth tip. Both unseeded and seeded growths were performed with total material charges up to 400 g. After the loading of starting CdZnTe material, a typical amount of 2 g of Cd was also loaded inside a Cd reservoir basket, which was attached beneath the seal-off cup. The ampoule was sealed off under a vacuum below lxl0(exp -5) Torr. The sealed ampoule was placed inside a 4-zone Bridgman furnace - a Cd reservoir zone with a heat-pipe furnace liner on the top, followed by a hot zone, a booster heating zone and a cold zone at the bottom. The Cd zone was typically 300 to 400 C below the hot zone setting. High resistivity material has been obtained without any intentional dopants but has been reproducibly obtained with In doping. The crystalline and the electrical properties of the crystals will be reported.

The modeling, simulation, and control of transport phenomena in a thermally destabilizing Bridgman crystal growth system

NASA Astrophysics Data System (ADS)

Sonda, Paul Julio

This thesis presents a comprehensive examination of the modeling, simulation, and control of axisymmetric flows occurring in a vertical Bridgman crystal growth system with the melt underlying the crystal. The significant complexity and duration of the manufacturing process make experimental optimization a prohibitive task. Numerical simulation has emerged as a powerful tool in understanding the processing issues still prevalent in industry. A first-principles model is developed to better understand the transport phenomena within a representative vertical Bridgman system. The set of conservation equations for momentum, energy, and species concentration are discretized using the Galerkin finite element method and simulated using accurate time-marching schemes. Simulation results detail the occurrence of fascinating nonlinear dynamics, in the form of stable, time-varying behavior for sufficiently large melt regimes and multiple steady flow states. This discovery of time-periodic flows for high intensity flows is qualitatively consistent with experimental observations. Transient simulations demonstrate that process operating conditions have a marked effect on the hydrodynamic behavior within the melt, which consequently affects the dopant concentration profile within the crystal. The existence of nonlinear dynamical behavior within this system motivates the need for feedback control algorithms which can provide superior crystal quality. This work studies the feasibility of using crucible rotation to control flows in the vertical Bridgman system. Simulations show that crucible rotation acts to suppress the axisymmetric flows. However, for the case when the melt lies below the crystal, crucible rotation also acts to accelerate the onset of time-periodic behavior. This result is attributed to coupling between the centrifugal force and the intense, buoyancy-driven flows. Proportional, proportional-integral, and input-output linearizing controllers are applied to vertical Bridgman systems in stabilizing (crystal below the melt) and destabilizing (melt below the crystal) configurations. The spatially-averaged, axisymmetric kinetic energy is the controlled output. The flows are controlled via rotation of the crucible containing the molten material. Simulation results show that feedback controllers using crucible rotation effectively attenuate flow oscillations in a stabilizing configuration with time-varying disturbance. Crucible rotation is not an optimal choice for suppressing inherent flow oscillations in the destabilizing configuration.

Optimization of the Bridgman crystal growth process

NASA Astrophysics Data System (ADS)

Margulies, M.; Witomski, P.; Duffar, T.

2004-05-01

A numerical optimization method of the vertical Bridgman growth configuration is presented and developed. It permits to optimize the furnace temperature field and the pulling rate versus time in order to decrease the radial thermal gradients in the sample. Some constraints are also included in order to insure physically realistic results. The model includes the two classical non-linearities associated to crystal growth processes, the radiative thermal exchange and the release of latent heat at the solid-liquid interface. The mathematical analysis and development of the problem is shortly described. On some examples, it is shown that the method works in a satisfactory way; however the results are dependent on the numerical parameters. Improvements of the optimization model, on the physical and numerical point of view, are suggested.

Numerical investigation on the batch characteristics of liquid encapsulated vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Lan, C. W.; Ting, C. C.

1995-04-01

Since the liquid encapsulated vertical Bridgman (LEVB) crystal growth is a batch process, it is time dependent in nature. A numerical simulation is conducted to study the unsteady features of the process, including the dynamic evolution of heat flow, growth rate, and interface morphology during crystal growth. The numerical model, which is governed by time-dependent equations for momentum and energy transport, and the conditions for evolution of melt/crystal and melt/encapsulant interfaces, is approximated by a body-fitted coordinate finite-volume method. The resulting differential/algebraic equations are then solved by the ILU (0) preconditioned DASPK code. Sample calculations are mainly conducted for GaAs. Dynamic effects of some process parameters, such as the growth speed, the ambient temperature profile, and ampoule design, are illustrated through calculated results. Due to the heat of fusion release and time-dependent end effects, in some cases a near steady-state operation is not possible. The control of growth front by modifying the ambient temperature profile is also demonstrated. Calculations are also performed for a 4.8 cm diameter InP crystal. The calculated melt/seed interface shape is compared with the measured one from Matsumoto et al. [J. Crystal Growth 132 (1993) 348] and they are in good agreement.

Morphological stability and kinetics in crystal growth from vapors

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1990-01-01

The following topics are discussed: (1) microscopy image storage and processing system; (2) growth kinetics and morphology study with carbon tetrabromide; (3) photothermal deflection vapor growth setup; (4) bridgman growth of iodine single crystals; (5) vapor concentration distribution measurement during growth; and (6) Monte Carlo modeling of anisotropic growth kinetics and morphology. A collection of presentations and publications of these results are presented.

Crystal Growth and Fluid Mechanics Problems in Directional Solidification

NASA Technical Reports Server (NTRS)

Tanveer, S.; Baker, G. R.; Foster, M. R.

1996-01-01

An investigation of a more complete theoretical understanding of convection effects in a vertical Bridgman apparatus is described. The aim is to develop a clear understanding of scalings of various features of dendritic crystal growth in the case that both the surface energy and undercooling are small.

Control of fluid flow during Bridgman crystal growth using low-frequency vibrational stirring

NASA Astrophysics Data System (ADS)

Zawilski, Kevin Thomas

The goal of this research program was to develop an in depth understanding of a promising new method for stirring crystal growth melts called coupled vibrational stirring (CVS). CVS is a mixing technique that can be used in sealed systems and produces rapid mixing through vortex flows. Under normal operating conditions, CVS uses low-frequency vibrations to move the growth crucible along a circular path, producing a surface wave and convection in the melt. This research focused on the application of CVS to the vertical Bridgman technique. CVS generated flows were directly studied using a physical modeling system containing water/glycerin solutions. Sodium nitrate was chosen as a model growth system because the growth process could be directly observed using a transparent furnace. Lead magnesium niobate-lead titanate (PMNT) was chosen as the third system because of its potential application for high performance solid state transducers and actuators. In this study, the critical parameters for controlling CVS flows in cylindrical Bridgman systems were established. One of the most important results obtained was the dependence of an axial velocity gradient on the vibrational frequency. By changing the frequency, the intensity of fluid flow at a given depth can be easily manipulated. The intensity of CVS flows near the crystal-melt interface was found to be important. When flow intensity near the interface increased during growth, large growth rate fluctuations and significant changes in interface shape were observed. To eliminate such fluctuations, a constant flow rate near the crystal-melt interface was maintained by decreasing the vibrational frequency. A continuous frequency ramp was found to be essential to grow crystals of good quality under strong CVS flows. CVS generated flows were also useful in controlling the shape of the growth interface. In the sodium nitrate system without stirring, high growth rates produced a very concave interface. By adjusting the flow intensity near the interface, CVS flows were able to flatten the growth interface under these extreme growth conditions.

Investigation of temperature and concentration oscillations in the directional solidification of Pb-Sn-Te

NASA Technical Reports Server (NTRS)

Anderson, T. J.; Narayanan, R.

1987-01-01

Directional solidification of the pseudobinary compound semiconductor material Pb sub 1-x Sn sub x Te by the Bridgman crystal growth process will be studied. Natural convection in the molten sample will be visualized with a novel electrochemical cell technique that employs the solid electrolyte material yttria-stabilized zirconia. Mass transfer by both diffusion and convection will be measured by detecting the motion of oxygen tracer in the liquid. Additional applications for electrochemical cells in semiconductor crystal growth are suggested. Unsteady convection in the melt will also be detected by the appearance of temperature oscillations. The purpose of this study is to experimentally characterize the overstable conditions for a Pb sub 1-x Sn sub x Te melt in the vertical Bridgman crystal growth technique and use a linear analysis to predict the onset of convection for this system.

Identification and Control of Gravity Related Defect Formation During Melt Growth of Electro-Optic Single Crystals Bismuth Silicate(Bi12SiO20)

NASA Technical Reports Server (NTRS)

Becia, Piotr; Wiegel, Michaela E. K.

2004-01-01

A research carried out under Award Number NAG8-1487 was aimed at to the design, conduct and analysis of experiments directed at the identification and control of gravitational effects on crystal growth, segregation and defect formation in the Sillenite system: bismuth silicate (Bi(12)SiO(20)). Correlation analyses was conducted in order to establish the influence of gravity related defects introduced during crystal growth on critical, application specific properties. Achievement of the states objective was conducted during the period from Feb. 01, 1998 to Dec. 31, 2003 with the following anticipated milestones: 1. Establishment of capabilities for (a) reproducible Czochralski and Bridgman-type growth of BSO single crystals and (b) for comprehensive analysis of crystalline and chemical defects as well as for selective property characterization of grown crystals (year 1). 2. Design and execution of critical space growth experiment(s) based on analyses of prefatory space results (experiments aimed at establishing the viability of planned approaches and procedures) and on unresolved issues related to growth, segregation and defect formation associated with conventional growth in Bridgman geometries. Comparative analysis of growth under conventional and under mu-g conditions; identification of gravity related defect formation during conventional Bridgman growth and formulation of approaches for their control (years 2 and 3). Development of charge confinement system which permits growth interface demarcation (in a mu-g environment) as well as minimization of confinement related stress and contamination during growth; design of complementary mu-g growth experiments aimed at quantitative mu-g growth and segregation analyses (year 4). 3. Conduct of quantitative mu-g growth experiments directed at: (a) identification and control of gravity related crystalline and chemical defect formation during single crystal growth of Bi(12)SiO(20) and at (b) defect engineering -the development of approaches to the controlled generation during crystal growth of specified point defects in homogeneous distribution (year 5). The proposed research places focus on a class of materials which have outstanding electrical and optical properties but have so far failed to reach their potential, primarily because of our inability to control adequately their stoichiometry and crystal defect formation as well as confinement related contamination and lattice stress.

Improving the growth of CZT crystals for radiation detectors: a modeling perspective

NASA Astrophysics Data System (ADS)

Derby, Jeffrey J.; Zhang, Nan; Yeckel, Andrew

2012-10-01

The availability of large, single crystals of cadmium zinc telluride (CZT) with uniform properties is key to improving the performance of gamma radiation detectors fabricated from them. Towards this goal, we discuss results obtained by computational models that provide a deeper understanding of crystal growth processes and how the growth of CZT can be improved. In particular, we discuss methods that may be implemented to lessen the deleterious interactions between the ampoule wall and the growing crystal via engineering a convex solidification interface. For vertical Bridgman growth, a novel, bell-curve furnace temperature profile is predicted to achieve macroscopically convex solid-liquid interface shapes during melt growth of CZT in a multiple-zone furnace. This approach represents a significant advance over traditional gradient-freeze profiles, which always yield concave interface shapes, and static heat transfer designs, such as pedestal design, that achieve convex interfaces over only a small portion of the growth run. Importantly, this strategy may be applied to any Bridgman configuration that utilizes multiple, controllable heating zones. Realizing a convex solidification interface via this adaptive bell-curve furnace profile is postulated to result in better crystallinity and higher yields than conventional CZT growth techniques.

Estimation of the curvature of the solid liquid interface during Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Barat, Catherine; Duffar, Thierry; Garandet, Jean-Paul

1998-11-01

An approximate solution for the solid/liquid interface curvature due to the crucible effect in crystal growth is derived from simple heat flux considerations. The numerical modelling of the problem carried out with the help of the finite element code FIDAP supports the predictions of our analytical expression and allows to identify its range of validity. Experimental interface curvatures, measured in gallium antimonide samples grown by the vertical Bridgman method, are seen to compare satisfactorily to analytical and numerical results. Other literature data are also in fair agreement with the predictions of our models in the case where the amount of heat carried by the crucible is small compared to the overall heat flux.

Development of model-based control for Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Sonda, Paul; Yeckel, Andrew; Daoutidis, Prodromos; Derby, Jeffrey. J.

2004-05-01

We study the feasibility of using crucible rotation with feedback control to suppress oscillatory flows in two prototypical vertical Bridgman crystal growth systems—a stabilizing configuration driven by a time-oscillatory furnace disturbance and a thermally destabilized configuration, which exhibits inherent time-varying flows. Proportional controllers are applied to the two systems, with volume-averaged flow speed chosen as the single controlled output and crucible rotation chosen as the manipulated input. Proportional control is able to significantly suppress oscillations in the stabilizing configuration. For the destabilized case, control is effective for small-amplitude flows but is generally ineffective, due to the exacerbating effect of crucible rotation on the time-dependent flows exhibited by this system.

Growth of Ca 4YO(BO 3) 3 crystals by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Luo, Jun; Fan, Shiji; Wang, Jinchang; Zhong, Zhenwu; Qian, Guoxing; Sun, Renying

2001-07-01

Growth of single crystals of Ca 4YO(BO 3) 3 (YCOB) by the vertical Bridgman method is reported in this paper. By using near-sealed Pt crucibles to prevent volatilization of B 2O 3, the high-optical-quality YCOB crystals of 25 mm diameter and more than 40 mm in length have been grown at the furnace temperature of 50-80°C above the melting point of YCOB and the crucible lowering rates of 0.2-0.6 mm/h. Owing to the low vertical and radial temperature gradient, crack-free YCOB crystals have been obtained in the <0 1 0> and <0 0 1> directions. At the top of a YCOB boule, the dislocation density was found to decrease from the center to the outer area, and the average dislocation density is about 600/cm 2.

Mathematical model for the Bridgman-Stockbarger crystal growing system

NASA Technical Reports Server (NTRS)

Roberts, G. O.

1986-01-01

In a major technical breakthrough, a computer model for Bridgman-Stockbarger crystal growth was developed. The model includes melt convection, solute effects, thermal conduction in the ampule, melt, and crystal, and the determination of the curved moving crystal-melt interface. The key to the numerical method is the use of a nonuniform computational mesh which moves with the interface, so that the interface is a mesh surface. In addition, implicit methods are used for advection and diffusion of heat, concentration, and vorticity, for interface movement, and for internal gracity waves. This allows large time-steps without loss of stability or accuracy. Numerical results are presented for the interface shape, temperature distribution, and concentration distribution, in steady-state crystl growth. Solutions are presented for two test cases using water, with two different salts in solution. The two diffusivities differ by a factor of ten, and the concentrations differ by a factor of twenty.

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

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

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

2014-04-24

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

Stabilizing detached Bridgman melt crystal growth: Model-based nonlinear feedback control

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; Daoutidis, Prodromos; Derby, Jeffrey J.

2012-12-01

The dynamics and operability limits of a nonlinear-proportional-integral controller designed to stabilize detached vertical Bridgman crystal growth are studied. The manipulated variable is the pressure difference between upper and lower vapor spaces, and the controlled variable is the gap width at the triple-phase line. The controller consists of a model-based nonlinear component coupled with a standard proportional-integral controller. The nonlinear component is based on a capillary model of shape stability. Perturbations to gap width, pressure difference, wetting angle, and growth angle are studied under both shape stable and shape unstable conditions. The nonlinear-PI controller allows a wider operating range of gain than a standard PI controller used alone, is easier to tune, and eliminates solution multiplicity from closed-loop operation.

Interface Shape Control Using Localized Heating during Bridgman Growth

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Aggarwal, M. D.; Croll, A.

2008-01-01

Numerical calculations were performed to assess the effect of localized radial heating on the melt-crystal interface shape during vertical Bridgman growth. System parameters examined include the ampoule, melt and crystal thermal conductivities, the magnitude and width of localized heating, and the latent heat of crystallization. Concave interface shapes, typical of semiconductor systems, could be flattened or made convex with localized heating. Although localized heating caused shallower thermal gradients ahead of the interface, the magnitude of the localized heating required for convexity was less than that which resulted in a thermal inversion ahead of the interface. A convex interface shape was most readily achieved with ampoules of lower thermal conductivity. Increasing melt convection tended to flatten the interface, but the amount of radial heating required to achieve a convex interface was essentially independent of the convection intensity.

Models of Mass Transport During Microgravity Crystal Growth of Alloyed Semiconductors in a Magnetic Field

NASA Technical Reports Server (NTRS)

Ma, Nancy

2003-01-01

Alloyed semiconductor crystals, such as germanium-silicon (GeSi) and various II-VI alloyed crystals, are extremely important for optoelectronic devices. Currently, high-quality crystals of GeSi and of II-VI alloys can be grown by epitaxial processes, but the time required to grow a certain amount of single crystal is roughly 1,000 times longer than the time required for Bridgman growth from a melt. Recent rapid advances in optoelectronics have led to a great demand for more and larger crystals with fewer dislocations and other microdefects and with more uniform and controllable compositions. Currently, alloyed crystals grown by bulk methods have unacceptable levels of segregation in the composition of the crystal. Alloyed crystals are being grown by the Bridgman process in space in order to develop successful bulk-growth methods, with the hope that the technology will be equally successful on earth. Unfortunately some crystals grown in space still have unacceptable segregation, for example, due to residual accelerations. The application of a weak magnetic field during crystal growth in space may eliminate the undesirable segregation. Understanding and improving the bulk growth of alloyed semiconductors in microgravity is critically important. The purpose of this grant to to develop models of the unsteady species transport during the bulk growth of alloyed semiconductor crystals in the presence of a magnetic field in microgravity. The research supports experiments being conducted in the High Magnetic Field Solidification Facility at Marshall Space Flight Center (MSFC) and future experiments on the International Space Station.

Growth of binary organic NLO crystals: m.NA-p.NA and m.NA-CNA system

NASA Technical Reports Server (NTRS)

Singh, N. B.; Henningsen, T.; Hopkins, R. H.; Mazelsky, R.

1993-01-01

Experiments were carried out to grow 3.Nitroaniline (m.NA) crystals doped with 4.Nitroaniline (p.NA) and 2.chloro 4.Nitroaniline (CNA). The measured undercooling for m.NA, p.NA, and CNA were 0.21 tm K, 0.23 tm K, and 0.35 tm K respectively, where tm represents the melting temperature of the pure component. Because of the crystals' large heat of fusion and large undercooling, it was not possible to grow good quality crystals with low thermal gradients. In the conventional two-zone Bridgman furnace we had to raise the temperature of the hot zone above the decomposition temperature of CNA, p.NA, and m.NA to achieve the desired thermal gradient. To avoid decomposition, we used an unconventional Bridgman furnace. Two immiscible liquids, silicone oil and ethylene glycol, were used to build a special two-zone Bridgman furnace. A temperature gradient of 18 K/cm was achieved without exceeding the decomposition temperature of the crystal. The binary crystals, m.NA-p.NA and m.NA-CNA, were grown in centimeter size in this furnace. X-ray and optical characterization showed good optical quality.

Interface shapes during vertical Bridgman growth of (Pb, Sn)Te crystals

NASA Technical Reports Server (NTRS)

Huang, YU; Debnam, William J.; Fripp, Archibald L.

1990-01-01

Melt-solid interfaces obtained during vertical Bridgman growth of (Pb, Sn)Te crystals were investigated with a quenching technique. The shapes of these interfaces, revealed by etching longitudinally cut sections, were correlated with the composition variations determined by EMPA. These experiments demonstrated that the interface shape can be changed from concave to convex by moving its location from the edge of the cold zone into the hot zone. The metallography and microsegregation near the melt-solid interface were analyzed in detail. A sharp change in composition above the interface indicated the existence of a diffusion boundary layer 40-90 microns thick. This small diffusion boundary layer is consistent with strong convective mixing in the (Pb, Sn)Te melt.

Three-dimensional analysis of flow and segregation in vertical Bridgman crystal growth under axial and transversal magnetic fields

NASA Astrophysics Data System (ADS)

Lan, C. W.; Lee, I. F.; Yeh, B. C.

2003-07-01

Three-dimensional simulation, both pseudo-steady and time-dependent states, is carried out to illustrate the effects of magnetic fields on the flow and segregation in a vertical Bridgman crystal growth. With an axial magnetic field in a perfectly vertical growth, the calculated results are in good agreement with those obtained by a two-dimensional axisymmetric model. The asymptotic scaling of flow damping is also consistent with the boundary layer approximation regardless to the magnetic orientation. Radial and axial segregations are further discussed concluding that radial segregation could be severe if the flow damping is not adequate. Moreover, there is a regime of enhanced global dopant mixing due to the flow stretching by the axial field. Accordingly, the transversal field is more effective in pushing the growth to the diffusion-controlled limit and suppressing the asymmetric global flow due to ampule tilting.

Effects of centrifugal acceleration on the flows and segregation in vertical Bridgman crystal growth with steady ampoule rotation

NASA Astrophysics Data System (ADS)

Lan, C. W.

2001-07-01

The effects of centrifugal acceleration on the flows and segregation in vertical Bridgman crystal growth with steady ampoule rotation are investigated through numerical simulation. The numerical model is based on the Boussinesq approximation in a rotating frame, and the fluid flow, heat and mass transfer, and the growth interface are solved simultaneously by a robust finite-volume/Newton method. The growth of gallium-doped germanium (GaGe) in the Grenoble furnace is adopted as an example. The calculated results at small Froude number (Fr<<1) are consistent with the previous prediction (Lan, J. Crystal growth 197 (1999) 983). However, at a high rotation speed or in reduced gravity, where the centrifugal acceleration becomes important (Fr˜1), the results are quite different due to the secondary flow induced. Since the direction of the induced flow is different from that of the buoyancy convection due to the concave interface, the flow damping is more effective than that due to the Coriolis force alone. More importantly, radial segregation can be reversed during the flow transition from one to the other.

Stabilizing detached Bridgman melt crystal growth: Proportional-integral feedback control

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; Daoutidis, Prodromos; Derby, Jeffrey J.

2012-10-01

The dynamics, operability limits, and tuning of a proportional-integral feedback controller to stabilize detached vertical Bridgman crystal growth are analyzed using a capillary model of shape stability. The manipulated variable is the pressure difference between upper and lower vapor spaces, and the controlled variable is the gap width at the triple-phase line. Open and closed loop dynamics of step changes in these state variables are analyzed under both shape stable and shape unstable growth conditions. Effects of step changes in static contact angle and growth angle are also studied. Proportional and proportional-integral control can stabilize unstable growth, but only within tight operability limits imposed by the narrow range of allowed meniscus shapes. These limits are used to establish safe operating ranges of controller gain. Strong nonlinearity of the capillary model restricts the range of perturbations that can be stabilized, and under some circumstances, stabilizes a spurious operating state far from the set point. Stabilizing detachment at low growth angle proves difficult and becomes impossible at zero growth angle.

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Cobb, S. D.; Schweizer, M.; Walker, J. S.

2005-01-01

A series of (100)-oriented gallium-doped germanium crystals has been grown by the vertical Bridgman method and under the influence of a rotating magnetic field (RMF). Time-dependent flow instabilities occur when the critical magnetic Taylor number (Tm(sup c)) is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. Tm(sup c) decreases as the aspect ratio of the melt increases, and approaches the theoretical limit expected for an infinite cylinder. Intentional interface demarcations are introduced by pulsing the RMF on and off The RMF has a marked affect on the interface shape, changing it from concave to nearly flat as the RMF strength is increased.

Bridgman-type apparatus for the study of growth-property relationships - Arsenic vapor pressure-GaAs property relationship

NASA Technical Reports Server (NTRS)

Parsey, J. M.; Nanishi, Y.; Lagowski, J.; Gatos, H. C.

1982-01-01

A precision Bridgman-type apparatus is described which was designed and constructed for the investigation of relationships between crystal growth parameters and the properties of GaAs crystals. Several key features of the system are highlighted, such as the use of a heat pipe for precise arsenic vapor pressure control and seeding without the presence of a viewing window. Pertinent growth parameters, such as arsenic source temperature, thermal gradients in the growing crystal and in the melt, and the macroscopic growth velocity can be independently controlled. During operation, thermal stability better than + or - 0.02 C is realized; thermal gradients can be varied up to 30 C/cm in the crystal region, and up to 20 C/cm in the melt region; the macroscopic growth velocity can be varied from 50 microns/hr to 6.0 cm/hr. It was found that the density of dislocations depends critically on As partial pressure; and essentially dislocation-free, undoped, crystals were grown under As pressure precisely controlled by an As source maintained at 617 C. The free carrier concentration varied with As pressure variations. This variation in free carrier concentration was found to be associated with variations in the compensation ratio rather than with standard segregation phenomena.

Development and melt growth of novel scintillating halide crystals

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Yokota, Yuui; Shoji, Yasuhiro; Kral, Robert; Kamada, Kei; Kurosawa, Shunsuke; Ohashi, Yuji; Arakawa, Mototaka; Chani, Valery I.; Kochurikhin, Vladimir V.; Yamaji, Akihiro; Andrey, Medvedev; Nikl, Martin

2017-12-01

Melt growth of scintillating halide crystals is reviewed. The vertical Bridgman growth technique is still considered as very popular method that enables production of relatively large and commercially attractive crystals. On the other hand, the micro-pulling-down method is preferable when fabrication of small samples, sufficient for preliminary characterization of their optical and/or scintillation performance, is required. Moreover, bulk crystal growth is also available using the micro-pulling-down furnace. The examples of growths of various halide crystals by industrially friendly melt growth techniques including Czochralski and edge-defined film-fed growth methods are also discussed. Finally, traveling molten zone growth that in some degree corresponds to horizontal zone melting is briefly overviewed.

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

NASA Astrophysics Data System (ADS)

Lenin, M.; Ramasamy, P.

2008-10-01

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

An axial temperature profile curvature criterion for the engineering of convex crystal growth interfaces in Bridgman systems

NASA Astrophysics Data System (ADS)

Peterson, Jeffrey H.; Derby, Jeffrey J.

2017-06-01

A unifying idea is presented for the engineering of convex melt-solid interface shapes in Bridgman crystal growth systems. Previous approaches to interface control are discussed with particular attention paid to the idea of a "booster" heater. Proceeding from the idea that a booster heater promotes a converging heat flux geometry and from the energy conservation equation, we show that a convex interface shape will naturally result when the interface is located in regions of the furnace where the axial thermal profile exhibits negative curvature, i.e., where d2 T / dz2 < 0 . This criterion is effective in explaining prior literature results on interface control and promising for the evaluation of new furnace designs. We posit that the negative curvature criterion may be applicable to the characterization of growth systems via temperature measurements in an empty furnace, providing insight about the potential for achieving a convex interface shape, without growing a crystal or conducting simulations.

Growth rates and interface shapes in germanium and lead tin telluride observed in-situ, real-time in vertical Bridgman furnaces

NASA Technical Reports Server (NTRS)

Barber, P. G.; Berry, R. F.; Debnam, W. J.; Fripp, A. L.; Woodell, G.; Simchick, R. T.

1995-01-01

Using the advanced technology developed to visualize the melt-solid interface in low Prandtl number materials, crystal growth rates and interface shapes have been measured in germanium and lead tin telluride semiconductors grown in vertical Bridgman furnaces. The experimental importance of using in-situ, real time observations to determine interface shapes, to measure crystal growth rates, and to improve furnace and ampoule designs is demonstrated. The interface shapes observed in-situ, in real-time were verified by quenching and mechanically induced interface demarcation, and they were also confirmed using machined models to ascertain the absence of geometric distortions. Interface shapes depended upon the interface position in the furnace insulation zone, varied with the nature of the crystal being grown, and were dependent on the extent of transition zones at the ends of the ampoule. Actual growth rates varied significantly from the constant translation rate in response to the thermophysical properties of the crystal and its melt and the thermal conditions existing in the furnace at the interface. In the elemental semiconductor germanium the observed rates of crystal growth exceeded the imposed translation rate, but in the compound semiconductor lead tin telluride the observed rates of growth were less than the translation rate. Finally, the extent of ampoule thermal loading influenced the interface positions, the shapes, and the growth rates.

A modified Chang Brown model for the determination of the dopant distribution in a Bridgman Stockbarger semiconductor crystal growth system

NASA Astrophysics Data System (ADS)

Balint, A. M.; Mihailovici, M. M.; Bãltean, D. G.; Balint, St.

2001-08-01

In this paper, we start from the Chang-Brown model which allows computation of flow, temperature and dopant concentration in a vertical Bridgman-Stockbarger semiconductor growth system. The modifications made by us concern the melt/solid interface. Namely, we assume that the phase transition does not take place on a flat mathematical surface, but in a thin region (the so-called precrystallization-zone), masking the crystal, where both phases, liquid and solid, co-exist. We deduce for this zone new effective equations which govern flow, heat and dopant transport and make the coupling of these equations with those governing the same phenomena in the pure melt. We compute flow, temperature and dopant concentration for crystal and melt with thermophysical properties similar to gallium-doped germanium using the modified Chang-Brown model and compare the results to those obtained using the Chang-Brown model.

Experimental determination and numerical modelling of solid liquid interface shapes for vertical Bridgman grown GaSb crystals

NASA Astrophysics Data System (ADS)

Boiton, P.; Giacometti, N.; Santailler, J. L.; Duffar, T.; Nabot, J. P.

1998-11-01

A facility, based on a profiled resistive heater, has been designed for the growth of antimonide crystals (GaSb, InSb) by the vertical Bridgman method. Solid-liquid interface shapes during the growth of 2-in diameter crystals are marked by means of variations of the pulling rate and are revealed by chemical etching. The comparison with the calculated interface shapes, obtained using a finite element method, gives a satisfactory agreement. It is shown that the heat transfer and consequently the interface shapes are greatly influenced by the crucible assembly. For example, small spacings around the crucible or slots in the crucible holder can change the interface curvature from convex to concave. From numerical simulations it is also shown that convection in the melt flattens the interface but that an increase of the pulling rate has the reverse effect.

TlBr purification and single crystal growth for the detector applications

NASA Astrophysics Data System (ADS)

Kozlov, Vasilij; Heikkilä, Mikko; Kostamo, Pasi; Lipsanen, Harri; Leskelä, Markku

2011-05-01

The combination of distillation, Bridgman-Stockbarger, hydrothermal recrystallisation and travelling molten zone (TMZ) methods were used for TlBr purification. Grown crystals were characterised by XRD rocking curve and FTIR spectroscopy methods, and by electrical measurements made from 200 to 300 K.

The effect of growth rate on the compositional variations in directionally solidified Hg(1-x)CdsubxSe

NASA Technical Reports Server (NTRS)

Andrews, R. N.

1986-01-01

Several Hg1-xCdxSe crystals of composition x = 0.2 were grown in a bridgman-type directional solidification furnace at varying translation rates. The influence of growth rate on both the longitudinal and radial compositional uniformity for the crystals was determined using density measurements and infrared transmission-edge mapping.

Eddy current sensor concepts for the Bridgman growth of semiconductors

NASA Astrophysics Data System (ADS)

Dharmasena, Kumar P.; Wadley, Haydn N. G.

1997-03-01

Electromagnetic finite element methods have been used to identify eddy current sensor designs for monitoring CdTe vertical Bridgman crystal growth. A model system consisting of pairs of silicon cylinders with electrical conductivities similar to those of solid and liquid CdTe has been used to evaluate the multifrequency response of several sensors designed for locating and characterizing the curvature of liquid-solid interfaces during vertical Bridgman growth. At intermediate frequencies (100-800 kHz), the sensor's imaginary impedance monotonically increases as interfacial curvature changes from concave to convex or the interface location moves upwards through the sensor. The experimental data are in excellent agreement with theoretical predictions. At higher test frequencies (˜ 5 MHz), the test circuit's parasitics contribute to the sensor's response. Even so, the predicted trends with interface location/curvature were found to be still preserved, and the experiments confirm that the sensor's high frequency response depends more on interface location and has only a small sensitivity to curvature. Multifrequency data obtained from these types of sensors have the potential to separately discriminate the location and the shape of liquid-solid interfaces during the vertical Bridgman growth of CdTe and other semiconductor materials of higher electrical conductivity.

Advancing radiation balanced lasers (RBLs) in rare-earth (RE)-doped solids

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

Hehlen, Markus Peter

2016-11-21

These slides cover the following topics: Mid-IR lasers in crystals using two-tone RBL (Single-dopant two-tone RBLs: Tm 3+, Er 3+, and Co-doped two-tone RBLs: (Yb 3+, Nd 3+) and (Ho 3+, Tm 3+); Advanced approaches to RBL crystals (Precursor purification, Micro-pulling-down crystal growth, and Bridgman crystal growth); Advanced approaches to RBL fibers (Materials for RBL glass fibers, Micro-structured fibers for RBL, and Fiber preform synthesis); and finally objectives.

Inclusion free cadmium zinc tellurium and cadmium tellurium crystals and associated growth method

DOEpatents

Bolotnikov, Aleskey E [South Setauket, NY; James, Ralph B [Ridge, NY

2010-07-20

The present disclosure provides systems and methods for crystal growth of cadmium zinc tellurium (CZT) and cadmium tellurium (CdTe) crystals with an inverted growth reactor chamber. The inverted growth reactor chamber enables growth of single, large, high purity CZT and CdTe crystals that can be used, for example, in X-ray and gamma detection, substrates for infrared detectors, or the like. The inverted growth reactor chamber enables reductions in the presence of Te inclusions, which are recognized as an important limiting factor in using CZT or CdTe as radiation detectors. The inverted growth reactor chamber can be utilized with existing crystal growth techniques such as the Bridgman crystal growth mechanism and the like. In an exemplary embodiment, the inverted growth reactor chamber is a U-shaped ampoule.

Numerical analysis of melt-solid interface shapes and growth rates of gallium antimonide in a single-zone vertical Bridgman furnace

NASA Astrophysics Data System (ADS)

Dutta, P. S.; Bhat, H. L.; Kumar, Vikram

1995-09-01

Numerical analysis has been carried out to determine the deviation of the growth rate from the ampoule lowering rate and the shape of the isotherms during the growth of gallium antimonide using the vertical Bridgman technique in a single-zone furnace. Electrical analogues have been used to model the thermal behaviour of the growth system. The standard circuit analysis technique has been used to calculate the temperature distribution in the growing crystal under various growth conditions. The effects of furnace temperature gradient near the melt-solid interface, the ampoule lowering rate, the ampoule geometry, the thermal conductivity of the melt, the mode of heat extraction from the tip of the ampoule and the extent of lateral heat loss from the side walls of the ampoule on the shape of isotherms in the crystal have been evaluated. The theoretical results presented here agree well with our previously obtained experimental results.

Effect of accelerated crucible rotation on melt composition in high-pressure vertical Bridgman growth of cadmium zinc telluride

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; Derby, Jeffrey J.

2000-02-01

Three-dimensional axisymmetric, time-dependent simulations of the high-pressure vertical Bridgman growth of large-diameter cadmium zinc telluride are performed to study the effect of accelerated crucible rotation (ACRT) on crystal growth dynamics. The model includes details of heat transfer, melt convection, solid-liquid interface shape, and dilute zinc segregation. Application of ACRT greatly improves mixing in the melt, but causes an overall increased deflection of the solid-liquid interface. The flow exhibits a Taylor-Görtler instability at the crucible sidewall, which further enhances melt mixing. The rate of mixing depends strongly on the length of the ACRT cycle, with an optimum half-cycle length between 2 and 4 Ekman time units. Significant melting of the crystal occurs during a portion of the rotation cycle, caused by periodic reversal of the secondary flow at the solid-liquid interface, indicating the possibility of compositional striations.

Investigation of Artificial Forced Cooling in the Bridgman Crystal Growth of Cadmium Zinc Telluride

NASA Astrophysics Data System (ADS)

Liu, Juncheng; Li, Jiao; Zhang, Guodong; Li, Changxing; Lennon, Craig; Sivananthan, Siva

2007-08-01

The effects of artificial forced cooling on the solid liquid interface and on solute segregation were investigated by modeling the vertical Bridgman method for the single-crystal growth of CdZnTe, taking into consideration effects such as increasing the axial outward heat flux from the crucible bottom, the radial outward heat flux from the crucible wall, and the carbon film thickness on the crucible inner wall. Axial artificially forced cooling noticeably increases convection and the temperature gradient in the melt next to the solid liquid interface, and substantially reduces interface concavity at the initial solidification stage. Interface concavity increases a little when the solidification proceeds further, however. Axial artificially forced cooling reduces radial solute segregation of the initial segment of the grown crystal and slightly increases the solute iso-concentration segment. Radial artificially forced cooling enhances melt convection substantially, affects solid liquid interface concavity only slightly, and hardly affects solute segregation in the grown crystal. Doubling the carbon film thickness weakens convection of the melt in front of the interface, substantially increases interface concavity, and hardly affects solute segregation in the grown crystal.

Modelling of convective processes during the Bridgman growth of poly-silicon

NASA Astrophysics Data System (ADS)

Popov, V. N.

2009-09-01

An original 3D model was used to numerically examine convective heat-and-mass transfer processes in the melt during the growth of polycrystalline silicon in vertical Bridgman configuration. The flow in the liquid was modelled using the Navier — Stokes equations in the Boussinesq approximation. The distribution of dissolved impurities was determined by solving the convective diffusion equation. The effects due to non-uniform heating of the lateral wall of the vessel and due to the shape of the crystallization front on the structure of melt flows and on the distribution of dissolved impurities in the liquid are examined.

Bridgman growth and luminescence properties of dysprosium doped lead potassium niobate crystal

NASA Astrophysics Data System (ADS)

Liu, Wenbin; Tian, Tian; Yang, Bobo; Xu, Jiayue; Liu, Hongde

2017-06-01

Dy-doped lead potassium niobate (Pb2KNb5O15, PKN) single crystal was grown by the modified vertical Bridgman method through spontaneous nucleation. The crystal was brownish, transparent and inclusion free. Five excitation peaks of Dy3+ ions were clearly seen from near ultraviolet region to blue range. It was unique that the excitation peaks in blue range were more intense, especially the one centered at 455 nm. The emission bands consisted of blue, yellow and red emissions, which were at about 487 nm, 573 nm and 662 nm respectively. The CIE chromaticity diagram of PKN:Dy indicated that white light and yellow light could be emitted when the crystal was excited under near ultraviolet light and blue light, respectively. Thus PKN:Dy crystal is a candidate material whose emitting light could be tunable through changing the excited light wavelength.

Growth and characterization of SrI2:Eu2+ single crystal for gamma ray detector applications

NASA Astrophysics Data System (ADS)

Raja, A.; Daniel, D. Joseph; Ramasamy, P.; Singh, S. G.; Sen, S.; Gadkari, S. C.

2018-04-01

Europium activated Strontium Iodide single crystal was grown by vertical Bridgman-stockbarger technique. The melting point and freezing point of SrI2:Eu2+ crystal was analyzed by TG/DTA. The Radioluminescence emission was recorded. The scintillation measurement was carried out for the grown SrI2:Eu2+ crystal under 137Cs gamma energy source.

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

NASA Technical Reports Server (NTRS)

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

2002-01-01

A series of (100)-oriented gallium-doped germanium crystals have been grown by the Bridgman method and under the influence of a rotating magnetic field (RMF). The RMF has a marked affect on the interface shape, changing it from concave to nearly flat. The onset of time-dependent flow instabilities occurs when the critical magnetic Taylor number is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. The critical magnetic Taylor number is a sensitive function of the aspect ratio and, as the crystal grows under a constant applied magnetic field, the induced striations change from nonperiodic to periodic, undergo a period-doubling transition, and then cease to exist. Also, by pulsing the RMF on and off, it is shown that intentional interface demarcations can be introduced.

Studies on interface curvature during vertical Bridgman growth of InP in a flat-bottom container

NASA Astrophysics Data System (ADS)

Rudolph, P.; Matsumoto, F.; Fukuda, T.

1996-01-01

A simplified numerical simulation of the dynamic behaviour of the solid-liquid interface curvature during modified vertical Bridgman growth of 2 inch InP single crystals, in a flat-bottom container, with a seed of the same diameter is presented. The results agree with striation patterns observed by transmission X-ray topography. A nearly flat interface with slightly constant concavity has been ascertained in the front half of the grown ingots. It can be assumed that such a steady interface morphology is one of the basic requirements for the observed twin-free and reduced dislocation growth in this region. In an attempt to optimize the shape of the melting point isotherm in the last-to-freeze part of the crystals, the axial temperature gradient, the seed length, the growth velocity, the melt temperature and the conditions of heat transfer (different ambient atmospheres and plugs) as well as the temperature profile in the top region above the encapsulant have been varied in the model.

Bridgman Growth of GeSi Alloys in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Vujisic, L.; Motakef, S.

1998-01-01

Ge(0.95)Si(0.050 alloy crystals have been grown by the vertical Bridgman technique, both with and without an axial 5 Tesla magnetic field. The crystals were processed in a constant axial thermal gradient and the effects of graphite, hot pressed boron nitride, and pyrolitic boron nitride ampoule materials on interface shapes and macrosegregation profiles were investigated. The sample grown in a graphite ampoule at 5 Tesla exhibited a macroscopic axial concentration profile close to that of complete mixing and strong striation patterns. In samples grown in boron nitride ampoules, both with and without a 5 Tesla magnetic field applied, measured macroscopic axial concentration profiles were intermediate between those expected for a completely mixed melt and diffusion-controlled growth, and striation patterns were also observed. Possible explanations for the apparent inability of the magnetic field to reduce the flow velocities to below the growth velocities are discussed, and results of growth experiments in pyrolitic boron nitride ampoules are also described.

Influence of crucible support and radial heating on the interface shape during vertical Bridgman GaAs growth

NASA Astrophysics Data System (ADS)

Koai, K.; Sonnenberg, K.; Wenzl, H.

1994-03-01

Crucible assembly in a vertical Bridgman furnace is investigated by a numerical finite element model with the aim to obtain convex interfaces during the growth of GaAs crystals. During the growth stage of the conic section, a new funnel shaped crucible support has been found more effective than the concentric cylinders design similar to that patented by AT & T in promoting interface convexity. For the growth stages of the constant diameter section, the furnace profile can be effectively modulated by localized radial heating at the gradient zone. With these two features being introduced into a new furnace design, it is shown numerically that enhancement of interface convexity can be achieved using the presently available crucible materials.

Bridgman crystal growth

NASA Technical Reports Server (NTRS)

Carlson, Frederick

1990-01-01

The objective of this theoretical research effort was to improve the understanding of the growth of Pb(x)Sn(1-x)Te and especially how crystal quality could be improved utilizing the microgravity environment of space. All theoretical growths are done using the vertical Bridgman method. It is believed that improved single crystal yields can be achieved by systematically identifying and studying system parameters both theoretically and experimentally. A computational model was developed to study and eventually optimize the growth process. The model is primarily concerned with the prediction of the thermal field, although mass transfer in the melt and the state of stress in the crystal were of considerable interest. The evolution is presented of the computer simulation and some of the important results obtained. Diffusion controlled growth was first studied since it represented a relatively simple, but nontheless realistic situation. In fact, results from this analysis prompted a study of the triple junction region where the melt, crystal, and ampoule wall meet. Since microgravity applications were sought because of the low level of fluid movement, the effect of gravitational field strength on the thermal and concentration field was also of interest. A study of the strength of coriolis acceleration on the growth process during space flight was deemed necessary since it would surely produce asymmetries in the flow field if strong enough. Finally, thermosolutal convection in a steady microgravity field for thermally stable conditions and both stable and unstable solutal conditions was simulated.

Melt and metallic solution crystal growth of CuInSe 2

NASA Astrophysics Data System (ADS)

Baldus, A.; Benz, K. W.

1993-05-01

In this paper the fabrication of CuInSe 2 chalcopyrite single crystals by the vertical Bridgman technique using non-stoichiometric In 2Se 3-rich congruent composition and a novel ampoule design is describe. Furthermore the growth of CuInSe 2 crystals by the travelling heater method (THM) using an In solvent was investigated. The elemental composition of as-grown CuInSe 2 semiconducting compounds and their electrical properties are discussed and correlated with predictions made by an intrinsic chemistry model.

Microgravity crystal growth

NASA Technical Reports Server (NTRS)

2001-01-01

Advanced finite element models are used to study three-dimensional, time-dependent flow and segregation in crystal growth systems. In this image of a prototypical model for melt and crystal growth, pathlines at one instant in time are shown for the flow of heated liquid silicon in a cylindrical container. The container is subjected to g-jitter disturbances along the vertical axis. A transverse magnetic field is applied to control them. Such computations are extremely powerful for understanding melt growth in microgravity where g-jitter drives buoyant flows. The simulation is part of the Theoretical Analysis of 3D, Transient Convection and Segregation in Microgravity Bridgman Crystal Growth investigation by Dr. Jeffrey J. Derby of the University of Mirnesota, Minneapolis.

High resolution X-ray diffraction imaging of lead tin telluride

NASA Technical Reports Server (NTRS)

Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Spal, Richard; Simchick, Richard; Fripp, Archibald

1991-01-01

High resolution X-ray diffraction images of two directly comparable crystals of lead tin telluride, one Bridgman-grown on Space Shuttle STS 61A and the other terrestrially Bridgman-grown under similar conditions from identical material, present different subgrain structure. In the terrestrial, sample 1 the appearance of an elaborate array of subgrains is closely associated with the intrusion of regions that are out of diffraction in all of the various images. The formation of this elaborate subgrain structure is inhibited by growth in microgravity.

Bridgman Crystal Growth of an Alloy with Thermosolutal Convection Under Microgravity Conditions

NASA Technical Reports Server (NTRS)

Simpson, James E.; Garimella, Suresh V.; deGroh, Henry C., III; Abbaschian, Reza

2000-01-01

The solidification of a dilute alloy (bismuth-tin) under Bridgman crystal growth conditions is investigated. Computations are performed in two dimensions with a uniform grid. The simulation includes the species concentration, temperature and flow fields, as well as conduction in the ampoule. Fully transient simulations have been performed, with no simplifying steady state approximations. Results are obtained under microgravity conditions for pure bismuth, and for Bi-0.1 at.%Sn and Bi-1.0 at.%Sn alloys, and compared with experimental results obtained from crystals grown in the microgravity environment of space. For the Bi-1.0 at.%Sn case the results indicate that a secondary convective cell, driven by solutal gradients, forms near the interface. The magnitude of the velocities in this cell increases with time, causing increasing solute segregation at the solid/liquid interface. The concentration-dependence of the melting temperature is incorporated in the model for the Bi-1.0 at.%Sn alloy. Satisfactory correspondence is obtained between the predicted and experimental results in terms of solute concentrations in the solidified crystal.

Development of the vertical Bridgman technique for 6-inch diameter c-axis sapphire growth supported by numerical simulation

NASA Astrophysics Data System (ADS)

Miyagawa, Chihiro; Kobayashi, Takumi; Taishi, Toshinori; Hoshikawa, Keigo

2014-09-01

Based on the growth of 3-inch diameter c-axis sapphire using the vertical Bridgman (VB) technique, numerical simulations were made and used to guide the growth of a 6-inch diameter sapphire. A 2D model of the VB hot-zone was constructed, the seeding interface shape of the 3-inch diameter sapphire as revealed by green laser scattering was estimated numerically, and the temperature distributions of two VB hot-zone models designed for 6-inch diameter sapphire growth were numerically simulated to achieve the optimal growth of large crystals. The hot-zone model with one heater was selected and prepared, and 6-inch diameter c-axis sapphire boules were actually grown, as predicted by the numerical results.

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

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

Effect of steady crucible rotation on segregation in high-pressure vertical Bridgman growth of cadmium zinc telluride

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; Patrick Doty, F.; Derby, Jeffrey J.

1999-05-01

Three-dimensional axisymmetric, time-dependent simulations of the high-pressure vertical Bridgman growth of large-diameter cadmium zinc telluride are performed to study the effect of steady crucible rotation on axial and radial segregation in the grown crystal. The model includes details of heat transfer, melt convection, solid-liquid interface shape, and pseudo-binary zinc segregation. Imposing a moderate rotation rate of 10 rpm on the system slightly improves axial segregation but makes radial segregation much worse. Moreover, values of dimensionless thermal Rossby and Taylor numbers calculated for this system indicate that the baroclinic instability may occur at the rotation rates studied.

Bulk Crystal Growth of Nonlinear Optical Organic Materials Using Inverted Vertical Gradient Freeze Method

NASA Technical Reports Server (NTRS)

Choi, J.; Cruz, Magda; Metzl, R.; Wang, W. S.; Aggarwal, M. D.; Penn, Benjamin G.; Frazier, Donald O.

1998-01-01

A new process for producing large bulk single crystals of benzil (C6H5COCOC6H5) is reported in this paper. Good quality crystals have been successfully grown using this approach to crystal growth. This method seems to be very promising for other thermally stable NLO organic materials also. The entire contents vycor crucible 1.5 inch in diameter and 2 inch deep was converted to single crystal. Purity of the starting growth material is also an important factor in the final quality of the grown crystals. The entire crystal can be very easily taken out of the crucible by simple maneuvering. Initial characterization of the grown crystals indicated that the crystals are as good as other crystals grown by conventional Bridgman Stockbarger technique.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Astrophysics Data System (ADS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-09-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-01-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

NASA Technical Reports Server (NTRS)

Volz, M. P.; Walker, J. S.; Schweizer, M.; Cobb, S. D.; Szofran, F. R.

2004-01-01

A series of (100)-oriented gallium-doped germanium crystals have been grown by the Bridgman method and under the influence of a rotating magnetic field (RMF). Time-dependent flow instabilities occur when the critical magnetic Taylor number (Tm(sup c) is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. The experimental data indicate that Tm(sup c) increases as the aspect ratio of the melt decreases. Modeling calculations predicting Tm(sup c) as a function of aspect ratio are in reasonable agreement with the experimental data. The RMF has a marked affect on the interface shape, changing it from concave to nearly flat as the RMF strength is increased. Also, by pulsing the RMF on and off, it is shown that intentional interface demarcations can be introduced.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Benz, K. W.; Cobb, S. D.; Croell, A.; Dold, P.; Kaiser, N.; Motakel, S.; Walker, J. S.

2000-01-01

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached-Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur frequently during microg experiments and considerable improvements of crystal quality have been reported for those cases. However, no thorough understanding of the process or quantitative assessment of the quality improvements exists so far. This project is determining the means to reproducibly grow Ge-Si alloys in the detached mode.

Numerical modeling of crystal growth in Bridgman device

NASA Astrophysics Data System (ADS)

Vompe, Dmitry Aleksandrovich

1997-12-01

The standard model for the growth of a crystal from a pure substance or diluted binary mixture contains transport equations for heat and phase change conditions at the solidification front. A numerical method is constructed for simulations of crystal growth in a vertical Bridgman device. The method is based on a boundary fitting technique in which melted and solidified regions are mapped onto a fixed rectangular logical domain. The Alternating Directions scheme (ADI) is used to treat the diffusive terms implicitly, with explicit methods are used for the remaining terms in the mapped temperature equations with variable coefficients. The nonlinear equation for the solid/liquid interface motion is solved by the modified Euler technique. Results obtained from the calculations have been used to study the influence of various boundary conditions imposed on the sidewalls and the top and bottom of the ampoule. Conditions are identified that lead to a steadily growing crystal and results are compared with an asymptotic one- dimensional model. Criteria based on ampoule length and boundary conditions being derived and compared with a previously developed one-dimensional model. Various cases have been considered to determine conditions for maintaining a nearly flat interface. It was found that the interface amplitude can be decreased by a factor of 100 (even 1,000) by optimizing temperature boundary conditions.

Existence, stability, and nonlinear dynamics of detached Bridgman growth states under zero gravity

NASA Astrophysics Data System (ADS)

Yeckel, Andrew; Derby, Jeffrey J.

2011-01-01

A thermocapillary model is used to study the existence, stability, and nonlinear dynamics of detached melt crystal growth in a vertical Bridgman system under zero gravity conditions. The model incorporates time-dependent heat, mass, and momentum transport, and accounts for temperature-dependent surface tension effects at the menisci bounding the melt. The positions of the menisci and phase-change boundary are computed to satisfy the conservation laws rigorously. A rich bifurcation structure in gap width versus pressure difference is uncovered, demarcating conditions under which growth with a stable gap is feasible. Thermal effects shift the bifurcation diagram to a slightly different pressure range, but do not alter its general structure. Necking and freeze-off are shown to be two different manifestations of the same instability mechanism. Supercooling of melt at the meniscus and low thermal gradients in the melt ahead of the crystal-melt-gas triple phase line, either of which may be destabilizing, are both observed under some conditions. The role of wetting and growth angles in dynamic shape stability is clarified.

Bridgman growth and scintillation properties of calcium tungstate single crystal

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2017-06-01

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

Three-dimensional heat transfer effects during the growth of LiCaAlF 6 in a modified Bridgman furnace

NASA Astrophysics Data System (ADS)

Brandon, Simon; Derby, Jeffrey J.; Atherton, L. Jeffrey; Roberts, David H.; Vital, Russel L.

1993-09-01

A novel process modification, the simultaneous growth of three cylindrical Cr:LiCaAlf 6 (Cr:LiCAF) crystals grown from a common seed in a vertical Bridgman furnace of rectangular cross section, is assessed using computational modeling. The analysis employs the FIDAP finite-element package and accounts for three-dimensional, steady-state, conductive heat transfer throughout the system. The induction heating system is rigorously simulated via solution of Maxwell's equations. The implementation of realistic thermal boundary conditions and furnace details is shown to be important. Furnace design features are assessed through calculations, and simulations indicate expected growth conditions to be favorable. In addition, the validity of using ampoules containing "dummy" charges for experimental furnace characterization measurements is examined through test computations.

Real-time Crystal Growth Visualization and Quantification by Energy-Resolved Neutron Imaging.

PubMed

Tremsin, Anton S; Perrodin, Didier; Losko, Adrian S; Vogel, Sven C; Bourke, Mark A M; Bizarri, Gregory A; Bourret, Edith D

2017-04-20

Energy-resolved neutron imaging is investigated as a real-time diagnostic tool for visualization and in-situ measurements of "blind" processes. This technique is demonstrated for the Bridgman-type crystal growth enabling remote and direct measurements of growth parameters crucial for process optimization. The location and shape of the interface between liquid and solid phases are monitored in real-time, concurrently with the measurement of elemental distribution within the growth volume and with the identification of structural features with a ~100 μm spatial resolution. Such diagnostics can substantially reduce the development time between exploratory small scale growth of new materials and their subsequent commercial production. This technique is widely applicable and is not limited to crystal growth processes.

Real-time Crystal Growth Visualization and Quantification by Energy-Resolved Neutron Imaging

NASA Astrophysics Data System (ADS)

Tremsin, Anton S.; Perrodin, Didier; Losko, Adrian S.; Vogel, Sven C.; Bourke, Mark A. M.; Bizarri, Gregory A.; Bourret, Edith D.

2017-04-01

Energy-resolved neutron imaging is investigated as a real-time diagnostic tool for visualization and in-situ measurements of “blind” processes. This technique is demonstrated for the Bridgman-type crystal growth enabling remote and direct measurements of growth parameters crucial for process optimization. The location and shape of the interface between liquid and solid phases are monitored in real-time, concurrently with the measurement of elemental distribution within the growth volume and with the identification of structural features with a ~100 μm spatial resolution. Such diagnostics can substantially reduce the development time between exploratory small scale growth of new materials and their subsequent commercial production. This technique is widely applicable and is not limited to crystal growth processes.

Real-time Crystal Growth Visualization and Quantification by Energy-Resolved Neutron Imaging

PubMed Central

Tremsin, Anton S.; Perrodin, Didier; Losko, Adrian S.; Vogel, Sven C.; Bourke, Mark A.M.; Bizarri, Gregory A.; Bourret, Edith D.

2017-01-01

Energy-resolved neutron imaging is investigated as a real-time diagnostic tool for visualization and in-situ measurements of “blind” processes. This technique is demonstrated for the Bridgman-type crystal growth enabling remote and direct measurements of growth parameters crucial for process optimization. The location and shape of the interface between liquid and solid phases are monitored in real-time, concurrently with the measurement of elemental distribution within the growth volume and with the identification of structural features with a ~100 μm spatial resolution. Such diagnostics can substantially reduce the development time between exploratory small scale growth of new materials and their subsequent commercial production. This technique is widely applicable and is not limited to crystal growth processes. PMID:28425461

Growth of concentrated GaInSb alloys with improved chemical homogeneity at low and variable pulling rates

NASA Astrophysics Data System (ADS)

Stelian, C.; Duffar, T.; Mitric, A.; Corregidor, V.; Alves, L. C.; Barradas, N. P.

2005-09-01

Crystal growth of concentrated GaInSb alloys during vertical Bridgman method has been numerically and experimentally investigated. The numerical and experimental results show a strong solutal damping effect on the melt convection in the case of concentrated (x=0.1 and 0.2) alloys grown at 1 μm/s pulling rate of the crucible. This leads to a huge increase of chemical heterogeneities and solid-liquid interface curvature. Analytical relations, which describe the solutal effect on the melt convection, show that the damping effect can be avoided by using low growth rates. The experimental results for Bridgman solidification of Ga0.85In0.15Sb at V=0.4 μm/s pulling rate, show that the axial and radial variations of indium concentration in the sample are reduced as compared with crystals grown at high pulling rates. The interface deflection is maintained at lower values during the growth process and the morphological destabilization of the interface occurs only at the end of the solidification. The growth at variable pulling rates is also investigated and from the numerical modeling it is found that the axial chemical homogeneity of the sample can be improved.

Microgravity

NASA Image and Video Library

2001-01-24

Advanced finite element models are used to study three-dimensional, time-dependent flow and segregation in crystal growth systems. In this image of a prototypical model for melt and crystal growth, pathlines at one instant in time are shown for the flow of heated liquid silicon in a cylindrical container. The container is subjected to g-jitter disturbances along the vertical axis. A transverse magnetic field is applied to control them. Such computations are extremely powerful for understanding melt growth in microgravity where g-jitter drives buoyant flows. The simulation is part of the Theoretical Analysis of 3D, Transient Convection and Segregation in Microgravity Bridgman Crystal Growth investigation by Dr. Jeffrey J. Derby of the University of Mirnesota, Minneapolis.

Modeling effects of solute concentration in Bridgman growth of cadmium zinc telluride

NASA Astrophysics Data System (ADS)

Stelian, Carmen; Duffar, Thierry

2016-07-01

Numerical modeling is used to investigate the effect of solute concentration on the melt convection and interface shape in Bridgman growth of Cd1-x Znx Te (CZT). The numerical analysis is compared to experimental growth in cylindrical ampoules having a conical tip performed by Komar et al. (2001) [15]. In these experiments, the solidification process occurs at slow growth rate (V = 2 ṡ10-7 m / s) in a thermal field characterized by a vertical gradient GT = 20 K / cm at the growth interface. The computations performed by accounting the solutal effect show a progressive damping of the melt convection due to the depleted Zn at the growth interface. The computed shape of the crystallization front is in agreement with the experimental measurement showing a convex-concave shape for the growth through the conical part of the ampoule and a concave shape of the interface in the cylindrical region. The distribution of Zn is nearly uniform over the crystal length except for the end part of the ingots. The anomalous zinc segregation observed in some experiments is explained by introducing the hypothesis of incomplete charge mixing during the homogenization time which precedes the growth process. When the crystallization is started in ampoules having a very sharp conical tip, the heavy CdTe is accumulated at the bottom part of the melt, giving rise to anomalous segregation patterns, featuring very low zinc concentration in the ingots during the first stage of the solidification.

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

NASA Astrophysics Data System (ADS)

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

2008-01-01

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

Convection Induced by Traveling Magnetic Fields in Semiconductor Melts

NASA Technical Reports Server (NTRS)

Konstantin, Mazuruk

2000-01-01

Axisymmetric traveling magnetic fields (TMF) can be beneficial for crystal growth applications. such as the vertical Bridgman, float zone or traveling heater methods. TMF induces a basic flow in the form of a single roll. This type of flow can enhance mass and heat transfer to the growing crystal. More importantly, the TMF Lorentz body force induced in the system can counterbalance the buoyancy forces, so the resulting convection can be much smaller and even the direction of it can be changed. In this presentation, we display basic features of this novel technique. In particular, numerical calculations of the Lorentz force for arbitrary frequencies will be presented along with induced steady-state fluid flow profiles. Also, numerical modeling of the TMF counter-balancing natural convection in vertical Bridgman systems will be demonstrated.

Process modelling for space station experiments

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Alexander, J. Iwan D.

1988-01-01

The work performed during the first year 1 Oct. 1987 to 30 Sept. 1988 involved analyses of crystal growth from the melt and from solution. The particular melt growth technique under investigation is directional solidification by the Bridgman-Stockbarger method. Two types of solution growth systems are also being studied. One involves growth from solution in a closed container, the other concerns growth of protein crystals by the hanging drop method. Following discussions with Dr. R. J. Naumann of the Low Gravity Science Division at MSFC it was decided to tackle the analysis of crystal growth from the melt earlier than originally proposed. Rapid progress was made in this area. Work is on schedule and full calculations were underway for some time. Progress was also made in the formulation of the two solution growth models.

Numerical simulation of CdTe vertical Bridgman growth

NASA Astrophysics Data System (ADS)

Ouyang, Hong; Shyy, Wei

1997-04-01

Numerical simulation has been conducted for steady-state Bridgman growth of the CdTe crystal with two ampoule configurations, namely, flat base and semi-spherical base. The present model accounts for conduction, convection and radiation, as well as phase change dynamics. The enthalpy formulation for phase change has been incorporated into a pressure-based algorithm with multi-zone curvilinear grid systems. The entire system which consists of the furnace enclosure wall, the encapsulated gas and the ampoule, contains irregularly configured domains. To meet the competing needs of producing accurate solutions with reasonable computing resources, a two-level approach is employed. The present study reveals that although the two ampoule configurations are quite different, their influence on the melt-solid interface shape is modest, and the undesirable concave interface appears in both cases. Since the interface shape strongly depends on thermal conductivities between the melt and the crystal, as well as ampoule wall temperature, accurate prescriptions of materials transport properties and operating environment are crucial for successful numerical predictions.

Melt Convection Effects in the Bridgman Crystal Growth of an Alloy Under Microgravity Conditions

NASA Technical Reports Server (NTRS)

Simpson James E.; Garimella, Suresh V.; deGroh, Henry C., III; Abbaschian, Reza

1998-01-01

The solidification of a dilute bismuth-tin alloy under Bridgman crystal growth conditions is investigated in support of NASA's MEPHISTO space shuttle flight experiment. Computations are performed in two-dimensions with a uniform grid. The simulation includes the species-concentration, temperature and flow fields, as well as conduction in the ampoule. Fully transient simulations have been performed; no simplifying steady state approximations are used. Results are obtained under microgravity conditions for pure bismuth, and Bismuth-0.1 at.% Sn and Bi-1.0 at.% Sn alloys. The concentration dependence of the melting temperature is neglected; the solid/liquid interface temperature is assumed to be the melting temperature of pure bismuth for all cases studied. For the Bi-1.0 at.% Sn case the results indicate that a secondary convective cell, driven by solutal gradients, forms near the interface. The magnitude of the velocities in this cell increases with time; this causes increasing solute segregation at the liquid/solid interface.

A technique for measuring the heat transfer coefficient inside a Bridgman furnace

NASA Technical Reports Server (NTRS)

Rosch, W.; Jesser, W.; Debnam, W.; Fripp, A.; Woodell, G.; Pendergrass, T. K.

1993-01-01

Knowledge of the amount of heat that is conducted, advected and radiated between an ampoule and the furnace is important for understanding vertical Bridgman crystal growth. This heat transfer depends on the temperature, emissivities and geometries of both the furnace and ampoule, as well as the choice of ambient gas inside the furnace. This paper presents a method which directly measures this heat transfer without the need to know any physical properties of the furnace, the ampoule, or the gaseous environment. Data are given for one specific furnace in which this method was used.

Real-time Crystal Growth Visualization and Quantification by Energy-Resolved Neutron Imaging

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

Tremsin, Anton S.; Perrodin, Didier; Losko, Adrian S.

Energy-resolved neutron imaging is investigated as a real-time diagnostic tool for visualization and in-situ measurements of "blind" processes. This technique is demonstrated for the Bridgman-type crystal growth enabling remote and direct measurements of growth parameters crucial for process optimization. The location and shape of the interface between liquid and solid phases are monitored in real-time, concurrently with the measurement of elemental distribution within the growth volume and with the identification of structural features with a ~100 μm spatial resolution. Such diagnostics can substantially reduce the development time between exploratory small scale growth of new materials and their subsequent commercial production.more » This technique is widely applicable and is not limited to crystal growth processes.« less

Real-time Crystal Growth Visualization and Quantification by Energy-Resolved Neutron Imaging

DOE PAGES

Tremsin, Anton S.; Perrodin, Didier; Losko, Adrian S.; ...

2017-04-20

Energy-resolved neutron imaging is investigated as a real-time diagnostic tool for visualization and in-situ measurements of "blind" processes. This technique is demonstrated for the Bridgman-type crystal growth enabling remote and direct measurements of growth parameters crucial for process optimization. The location and shape of the interface between liquid and solid phases are monitored in real-time, concurrently with the measurement of elemental distribution within the growth volume and with the identification of structural features with a ~100 μm spatial resolution. Such diagnostics can substantially reduce the development time between exploratory small scale growth of new materials and their subsequent commercial production.more » This technique is widely applicable and is not limited to crystal growth processes.« less

The growth of homogeneous semiconductor crystals in a centrifuge by the stabilizing influence of the Coriolis force

NASA Astrophysics Data System (ADS)

Müller, G.; Neumann, G.; Weber, W.

1992-04-01

Both experimental and numerical results on crystal growth and fluid flow studies carried out in a centrifuge are reported. It is shown that the formation of doping striations can be avoided in the vertical Bridgman and the horizontal zone melting growth of Te-doped InSb if the centrifugal acceleration is increased beyond a critical value depending on the thermal boundary conditions. Furthermore, the maximum rate for the growth of inclusion free GaSb crystals grown by the travelling heater method (THM) is increased by a factor of 10 if this method is carried out at an acceleration of 20 times earth gravity. Model experiments in the Bridgman configuration using a test cell with liquid Ga and a larger series of thermocouples are conducted by varying the thermal boundary conditions and the rotation rate of the centrifuge. A three-dimensional time dependent numerical simulation of the fluid flow under the experimental conditions was carried out using a finite difference numerical scheme. It follows clearly that the Coriolis force acting on the melt in the rotating centrifuge system significantly influences the buoyancy-driven convection with respect to the flow patterns as well as the stability. The Coriolis force causes two very different flow states (I and II), depending on whether the rotation sense of the flow is in the same or in the opposite direction to that of the centrifuge. Type I is very similar to that normally observed on earth. Type II is only observed on the centrifuge and has a very large stability range of steady convection which can be used to grow striation-free crystals. All results give excellent agreement between model experiments and numerical calculations, which finally leads to a fully satisfying explanation of the crystal growth results on our centrifuge.

Investigation of Vibrational Control of the Bridgman Crystal Growth Technique

NASA Technical Reports Server (NTRS)

Fedoseyev, Alexandre I.; Alexander, J. I. D.; Feigelson, R. S.; Zharikov, E. V.; Ostrogorsky, A. G.; Marin, C.; Volz, M. P.; Kansa, E. J.; Friedman, M. J.

2001-01-01

The character of natural buoyant convection in rigidly contained inhomogeneous fluids can be drastically altered by vibrating the container. Vibrations are expected to play a crucial influence on heat and mass transfer onboard the International Space Station (ISS). It is becoming evident that substantial vibrations will exist on the ISS in the wide frequency spectrum. In general, vibrational flows are very complex and governed by many parameters. In many terrestrial crystal growth situations, convective transport of heat and constituent components is dominated by buoyancy driven convection arising from compositional and thermal gradients. Thus, it may be concluded that vibro-convective flow can potentially be used to influence and even control transport in some crystal growth situations.

Influence of Applied Thermal Gradients and a Static Magnetic Field on Bridgman-Grown GeSi Alloys

NASA Technical Reports Server (NTRS)

Volz, M. P.; Szofran, F. R.; Cobb, S. D.; Ritter, T. M.

1999-01-01

The effect of applied axial and radial thermal gradients and an axial static magnetic field on the macrosegregation profiles of Bridgman-grown GeSi alloy crystals has been assessed. The axial thermal gradients were adjusted by changing the control setpoints of a seven-zone vertical Bridgman furnace. The radial thermal gradients were affected by growing samples in ampoules with different thermal conductivities, namely graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN). Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. All of the samples were grown on Ge seeds. This resulted in a period of free growth until the Si concentration in the solid was in equilibrium with the Si concentration in the liquid. The length of crystal grown during this period was inversely proportional to the applied axial thermal gradient. Several samples were grown in an axial 5 Tesla magnetic field. Measured macroscopic segregation profiles on these samples indicate that the magnetic field did not, in general, reduce the melt flow velocities to below the growth velocities.

Divalent europium doped and un-doped calcium iodide scintillators: Scintillator characterization and single crystal growth

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

Boatner, L. A.; Ramey, J. O.; Kolopus, J. A.

2015-02-21

Initially, the alkaline-earth scintillator, CaI 2:Eu 2+, was discovered around 1964 by Hofstadter, Odell, and Schmidt. Serious practical problems quickly arose, however, that were associated with the growth of large monolithic single crystals of this material due to its lamellar, mica-like structure. As a result of its theoretically higher light yield, CaI 2:Eu 2+ has the potential to exceed the excellent scintillation performance of SrI 2:Eu 2+. In fact, theoretical predictions for the light yield of CaI2:Eu 2+ scintillators suggested that an energy resolution approaching 2% at 662 keV could be achievable. Like the early SrI 2:Eu 2+ scintillator, themore » performance of CaI 2:Eu 2+ scintillators has traditionally suffered due, at least in part, to outdated materials synthesis, component stoichiometry/purity, and single-crystal-growth techniques. Based on our recent work on SrI 2:Eu 2+ scintillators in single-crystal form, we have developed new techniques that are applied here to CaI 2:Eu 2+ and pure CaI 2 with the goal of growing large un-cracked crystals and, potentially, realizing the theoretically predicted performance of the CaI 2:Eu 2+ form of this material. Calcium iodide does not adhere to modern glassy carbon Bridgman crucibles - so there should be no differential thermal-contraction-induced crystal/crucible stresses on cooling that would result in crystal cracking of the lamellar structure of CaI 2. Here we apply glassy carbon crucible Bridgman growth, high-purity growth-charge compounds, our molten salt processing/filtration technique, and extended vacuum-melt-pumping methods to the growth of both CaI 2:Eu 2+ and un-doped CaI 2. Moreover, large scintillating single crystals were obtained, and detailed characterization studies of the scintillation properties of CaI 2:Eu 2+ and pure CaI 2 single crystals are presented that include studies of the effects of plastic deformation of the crystals on the scintillator performance.« less

On the behaviour and origin of the major deep level (EL2) in GaAs

NASA Technical Reports Server (NTRS)

Lagowski, J.; Parsey, J. M.; Kaminska, M.; Wada, K.; Gatos, H. C.

1982-01-01

In an extensive crystal growth and characterization study of Bridgman-grown GaAs it was established that the following factors affect the concentration of the EL2 level: (1) the As pressure during growth; (2) the partial pressure of Ga2O; (3) the concentration of shallow donors and acceptors; and (4) the post-growth cooling cycle. The role of these factors is qualitatively and quantitatively explained by attributing the 0.82 eV donor state to the antisite defect As-sub-Ga formed as a result of Ga-vacancy migration during the post-growth cooling of the crystals.

Experimental analysis and modeling of melt growth processes

NASA Astrophysics Data System (ADS)

Müller, Georg

2002-04-01

Melt growth processes provide the basic crystalline materials for many applications. The research and development of crystal growth processes is therefore driven by the demands which arise from these specific applications; however, common goals include an increased uniformity of the relevant crystal properties at the micro- and macro-scale, a decrease of deleterious crystal defects, and an increase of crystal dimensions. As melt growth equipment and experimentation becomes more and more expensive, little room remains for improvements by trial and error procedures. A more successful strategy is to optimize the crystal growth process by a combined use of experimental process analysis and computer modeling. This will be demonstrated in this paper by several examples from the bulk growth of silicon, gallium arsenide, indium phosphide, and calcium fluoride. These examples also involve the most important melt growth techniques, crystal pulling (Czochralski methods) and vertical gradient freeze (Bridgman-type methods). The power and success of the above optimization strategy, however, is not limited only to the given examples but can be generalized and applied to many types of bulk crystal growth.

Convection effects on radial segregation and crystal melt interface in vertical Bridgman growth

NASA Technical Reports Server (NTRS)

Tanveer, S.

1993-01-01

We analytically study the influence of convection caused by horizontal heat transfer through the sides of a vertical Bridgman apparatus. We consider the case when the heat transfer across the side walls is small so that the resulting interfacial deformation and fluid velocities are also small. This allows us to linearize the Navier-Stokes equations and express the interfacial conditions about a planar interface through a Taylor expansion. Using a no tangential stress conditions on the side walls, asymptotic expressions for both the interfacial slope, and radial segregation at the crystal-melt interface are obtained in closed form in the limit of large thermal Rayleigh number. It is suggested that these can be reduced by appropriately controlling a specific heat transfer property at the edge of the insulation zone in the solid side.

Experimental observation of the influence of furnace temperature profile on convection and segregation in the vertical Bridgman crystal growth technique

NASA Technical Reports Server (NTRS)

Neugebauer, G. T.; Wilcox, W. R.

1990-01-01

Azulene-doped naphtalene was directionally solidified using the vertical Bridgman-Stockbarger technique. Doping homogeneity and convection are determined as a function of the temperature profile in the furnace and the freezing rate. Convective velocities are two orders of magnitude lower when the temperature increases with height. The cross sectional variation in azulene concentration tends to be asymmetric. Neither rotation of the ampoule nor deliberate introduction of thermal asymmetries during solidification had a significant influence on cross sectional variations in doping. It is predicted that slow directional solidification under microgravity conditions can produce greater inhomogeneities than on earth. Thus when low freezing rates are necessary in order to avoid constitutional supercooling, it may be necessary to combine microgravity and magnetic fields in order to achieve homogeneous crystals.

Fluid mechanics and mass transfer in melt crystal growth: Analysis of the floating zone and vertical Bridgman processes

NASA Technical Reports Server (NTRS)

Brown, R. A.

1986-01-01

This research program focuses on analysis of the transport mechanisms in solidification processes, especially one of interest to the Microgravity Sciences and Applications Program of NASA. Research during the last year has focused on analysis of the dynamics of the floating zone process for growth of small-scale crystals, on studies of the effect of applied magnetic fields on convection and solute segregation in directional solidification, and on the dynamics of microscopic cell formation in two-dimensional solidification of binary alloys. Significant findings are given.

Purification of organic nonlinear optical materials for bulk crystal growth from melt

NASA Astrophysics Data System (ADS)

Gebre, Tesfaye; Bhat, Kamala N.; Batra, Ashok K.; Lal, Ravindra B.; Aggarwal, Mohan D.; Penn, Benjamin G.; Frazier, Donald O.

2002-10-01

The techniques developed for purification of nonlinear optical organic materials, such as benzil, 2-methyl-4-nitroaniline (MNA), Dicyanovinyl anisole (DIVA) and its derivatives, nitrophenyl prolinol (NPP) and other Schiff's base compounds, include Kugelrohy method, physical vapor transport, zone refining and recrystallization from the solvent are described. Purity of the materials is tested using differential thermal analysis, gas chromatograph/Mass detector, Fourier Transform Infrared spectroscopy and melting point measurements. The purified materials were later used in the growth of single crystal by Bridgman-Stockbarger and Czochralski techniques.

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

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

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

Growth of Bulk Wide Bandgap Semiconductor Crystals and Their Potential Applications

NASA Technical Reports Server (NTRS)

Chen, Kuo-Tong; Shi, Detang; Morgan, S. H.; Collins, W. Eugene; Burger, Arnold

1997-01-01

Developments in bulk crystal growth research for electro-optical devices in the Center for Photonic Materials and Devices since its establishment have been reviewed. Purification processes and single crystal growth systems employing physical vapor transport and Bridgman methods were assembled and used to produce high purity and superior quality wide bandgap materials such as heavy metal halides and II-VI compound semiconductors. Comprehensive material characterization techniques have been employed to reveal the optical, electrical and thermodynamic properties of crystals, and the results were used to establish improved material processing procedures. Postgrowth treatments such as passivation, oxidation, chemical etching and metal contacting during the X-ray and gamma-ray device fabrication process have also been investigated and low noise threshold with improved energy resolution has been achieved.

Influence of temperature oscillations on the interface velocity during Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Stelian, Carmen; Duffar, Thierry; Santailler, Jean-Louis; Nicoara, Irina

2002-04-01

The objective of this work is the study of the effect of thermal oscillations on the interface velocity in the vertical Bridgman configuration. In order to study this effect, a transient numerical simulation of the heat transfer and melt convection is performed in a simplified geometrical model. The relation between the thermal signal amplitude and the amplitude of the velocity oscillations is investigated. When the oscillation period is varied, an asymptotic evolution of the velocity oscillation amplitude, with a cut-off period, is observed. It is shown that latent heat of solidification has a huge effect on the velocity amplitude, but not on the cut-off frequency.

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

Advanced crystal growth techniques for thallium bromide semiconductor radiation detectors

NASA Astrophysics Data System (ADS)

Datta, Amlan; Becla, Piotr; Guguschev, Christo; Motakef, Shariar

2018-02-01

Thallium Bromide (TlBr) is a promising room-temperature radiation detector candidate with excellent charge transport properties. Currently, Travelling Molten Zone (TMZ) technique is widely used for growth of semiconductor-grade TlBr crystals. However, there are several challenges associated with this type of crystal growth process including lower yield, high thermal stress, and low crystal uniformity. To overcome these shortcomings of the current technique, several different crystal growth techniques have been implemented in this study. These include: Vertical Bridgman (VB), Physical Vapor Transport (PVT), Edge-defined Film-fed Growth (EFG), and Czochralski Growth (Cz). Techniques based on melt pulling (EFG and Cz) were demonstrated for the first time for semiconductor grade TlBr material. The viability of each process along with the associated challenges for TlBr growth has been discussed. The purity of the TlBr crystals along with its crystalline and electronic properties were analyzed and correlated with the growth techniques. Uncorrected 662 keV energy resolutions around 2% were obtained from 5 mm x 5 mm x 10 mm TlBr devices with virtual Frisch-grid configuration.

Numerical study of heat transfer and fluid flow for steady crystal growth in a vertical Bridgman device

NASA Astrophysics Data System (ADS)

Pohlman, Matthew Michael

The study of heat transfer and fluid flow in a vertical Bridgman device is motivated by current industrial difficulties in growing crystals with as few defects as possible. For example, Gallium Arsenide (GaAs) is of great interest to the semiconductor industry but remains an uneconomical alternative to silicon because of the manufacturing problems. This dissertation is a two dimensional study of the fluid in an idealized Bridgman device. The model nonlinear PDEs are discretized using second order finite differencing. Newton's method solves the resulting nonlinear discrete equations. The large sparse linear systems involving the Jacobian are solved iteratively using the Generalized Minimum Residual method (GMRES). By adapting fast direct solvers for elliptic equations with simple boundary conditions, a good preconditioner is developed which is essential for GMRES to converge quickly. Trends of the fluid flow and heat transfer for typical ranges of the physical parameters are determined. Also, the size of the terms in the mathematical model are found by numerical investigation, in order to find what terms are in balance as the physical parameters vary. The results suggest the plausibility of simpler asymptotic solutions.

Interface Shape and Convection During Solidification and Melting of Succinonitrile

NASA Technical Reports Server (NTRS)

Degroh, Henry C., III; Lindstrom, Tiffany

1994-01-01

An experimental study was conducted of the crystal growth of succinonitrile during solidification, melting, and no-growth conditions using a horizontal Bridgman furnace and square glass ampoule. For use as input boundary conditions to numerical codes, thermal profiles on the outside of the ampoule at five locations around its periphery were measured along the ampoule's length. Temperatures inside the ampoule were also measured. The shapes of the s/l interface in various two dimensional planes were quantitatively determined. Though interfaces were nondendritic and noncellular, they were not flat, but were highly curved and symmetric in only one unique longitudinal y-z plane (at x=O). The shapes of the interface were dominated by the primary longitudinal flow cell characteristic of shallow cavity flow in horizontal Bridgman; this flow cell was driven by the imposed furnace temperature gradient and caused a 'radical' thermal gradient such that the upper half of the ampoule was hotter than the bottom half. We believe that due to the strong convection, the release of latent heat does not significantly influence the thermal conditions near the interface. We hope that the interface shape and thermal data presented in this paper can be used to optimize crystal growth processes and validate numerical models.

[Growth of codoped CdWO4 crystals by Bridgman method and their optical spectra].

PubMed

Yu, Can; Xia, Hai-Ping; Wang, Dong-Jie; Chen, Hong-Bing

2011-09-01

The CdWO4 crystals with good quality in the size of Phi25 mm x 120 mm, doped with Co in 0.5% molar fraction in the raw composition, were grown by the Bridgman method by taking -70 degrees C x cm(-1) of solid-liquid interface and -0.50 mm x h(-1) growth rate. The crystal presents transparence and deep blue. The X-ray diffraction (XRD) was used to characterize the crystals. Three absorption peaks at 518, 564 and 655 nm respectively, which are attributed to the overlapping of 4 T1 (4F) --> 4A2 (4F) and 4 T1 (4F) --> 4 T1 (4P) of Co2+ octahedrons, and a wide band centered at 1 863 nm, which is attributed to 4Ti (4F) --> 4 T2 (4F), was observed. The absorption results indicated that the Co ions presented +2 valence in crystal and located within the distorted oxygen octahedrons. The crystal-field parameter D(q) and the Racah parameter B were estimated to be 990 and 726.3 cm(-1) respectively based on the absorption spectra. A fluorescence emission at 778 nm (4T1 (4P) --> 4 T1 (4F)) for codoped CdWO4 crystals was observed under excitation by 520 nm light. It can be deduced from the changes in absorption and emission intensity of different parts of crystal that the concentration of Co2+ ion in crystal increased along growing direction and the effective distribution coefficient of Co2+ ion in CdWO4 crystal is less than 1.

Evolution of the Shape of Detached GeSi Crystals in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2013-01-01

A series of GeSi crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. An objective of these experiments is to understand the mechanisms of detached Bridgman growth, a process in which a gap exists between the growing semiconductor crystal and the crucible wall. Crystals grown without wall contact have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. Numerical calculations are used to determine the conditions in which a gap can exist. According to crystal shape stability theory, only some of these gap widths will be dynamically stable. Beginning with a crystal diameter that differs from stable conditions, the transient crystal growth process is analyzed. In microgravity, dynamic stability depends only on capillary effects and is decoupled from heat transfer. Depending on the initial conditions and growth parameters, the crystal shape will evolve towards the crucible wall, towards a stable gap width, or towards the center of the crucible, collapsing the meniscus.

A unified analysis of solidification in Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Lu, Ming-Fang

2012-04-01

The simulation of multiphase solidification process can be handled by combining the VOF (Volume of Fluid) transport equation, in which the continuum mechanics model is used to simulate the melt/solid interface and the conservation of mass, momentum, and energy. Because the melt phase, the solid phase, and the melt/solid interface are controlled by a single control equation; if the enthalpy model based on porosity concept represents the processing of the phase transformation range, it is possible to solve the problem of phase transformation in the same way as solving the single-phase problem. Once the energy field of enthalpy for each step in time is resolved, the position of the interface can be precisely calculated with the use of VOF equation. This type of novel VOF method can be applied to find out the conditions of vertical Bridgman crystal growing located on the earth or under microgravity.

A unified analysis of solidification in Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Lu, Ming-Fang

2011-11-01

The simulation of multiphase solidification process can be handled by combining the VOF (Volume of Fluid) transport equation, in which the continuum mechanics model is used to simulate the melt/solid interface and the conservation of mass, momentum, and energy. Because the melt phase, the solid phase, and the melt/solid interface are controlled by a single control equation; if the enthalpy model based on porosity concept represents the processing of the phase transformation range, it is possible to solve the problem of phase transformation in the same way as solving the single-phase problem. Once the energy field of enthalpy for each step in time is resolved, the position of the interface can be precisely calculated with the use of VOF equation. This type of novel VOF method can be applied to find out the conditions of vertical Bridgman crystal growing located on the earth or under microgravity.

Czochralski and modified Bridgman-Stockbarger growth of pure, Cd 2+ and Nd 3+ doped benzil single crystals

NASA Astrophysics Data System (ADS)

Aggarwal, M. D.; Wang, W. S.; Tambwe, M.

1993-03-01

Pure, Cd2+ and Nd3+-doped benzil C6H5COCOC6H5 have been grown from melt using the Czochralski and modified Bridgman-Stockbarger methods. Angle-tuned second harmonic generation of pure benzil from Nd:YAG laser radiation of λ = 1.06 μm with a conversion efficiency η = I2w/Iw = 0.4% has been demonstrated. We have used a Nd:YAG pulse laser to measure the radiation damage threshold as 15.9 MW/cm2 (c-axis) and 23.9 MW/cm2 (a-axis) under the conditions that laser pulse width is 10 ns. Under the same conditions, the conversion efficiency of Nd3+ and Cd2+-doped benzil, η= I2w/Iw = 1.1%, has been demonstrated. The radiation threshold is higher than for pure benzil crystals.

Producibility improvements suggested by a validated process model of seeded CdZnTe vertical Bridgman growth

NASA Astrophysics Data System (ADS)

Larson, David J., Jr.; Casagrande, Louis G.; Di Marzio, Don; Levy, Alan; Carlson, Frederick M.; Lee, Taipao; Black, David R.; Wu, Jun; Dudley, Michael

1994-07-01

We have successfully validated theoretical models of seeded vertical Bridgman-Stockbarger CdZnTe crystal growth and post-solidification processing, using in-situ thermal monitoring and innovative material characterization techniques. The models predict the thermal gradients, interface shape, fluid flow and solute redistribution during solidification, as well as the distributions of accumulated excess stress that causes defect generation and redistribution. Data from the furnace and ampoule wall have validated predictions from the thermal model. Results are compared to predictions of the thermal and thermo-solutal models. We explain the measured initial, change-of-rate, and terminal compositional transients as well as the macrosegregation. Macro and micro-defect distributions have been imaged on CdZnTe wafers from 40 mm diameter boules. Superposition of topographic defect images and predicted excess stress patterns suggests the origin of some frequently encountered defects, particularly on a macro scale, to result from the applied and accumulated stress fields and the anisotropic nature of the CdZnTe crystal. Implications of these findings with respect to producibility are discussed.

TEM investigations on twin boundary structures of feathery crystals in aluminum alloys during Bridgman solidification

NASA Astrophysics Data System (ADS)

Yang, Luyan; Li, Shuangming; Fan, Kai; Li, Yang; Zhong, Hong; Fu, Hengzhi

2018-06-01

Feathery crystals are an ensemble of twinned dendrites, and are characterized by a unique twin boundary (TB) structure in the solidification pattern of aluminum alloys. In this work, the high-density twinned dendrites of Al-4.5 wt% Cu alloys, produced during the Bridgman solidification, have been studied using electron backscattered diffraction (EBSD) and high-resolution transmission electron microscopy (HRTEM). The experimental results showed that, after systematically decreasing the growth rate from 3000 μm/s to 1 μm/s, the TBs remained stable, while the solute field around the TBs changed significantly. According to the HRTEM results, successive stacking faults were occurred near the TBs at 1 μm/s, while slight distortion was observed around the TBs at 3000 μm/s. The composition analysis revealed an obvious solute enrichment near the TBs. Furthermore, the solute gradient profile within the TBs became smoother with the decrease in the growth speed. This is due to the more sufficient solid-state back diffusion occurring perpendicular to the twin plane after the solidification.

Novel casting processes for single-crystal turbine blades of superalloys

NASA Astrophysics Data System (ADS)

Ma, Dexin

2018-03-01

This paper presents a brief review of the current casting techniques for single-crystal (SC) blades, as well as an analysis of the solidification process in complex turbine blades. A series of novel casting methods based on the Bridgman process were presented to illustrate the development in the production of SC blades from superalloys. The grain continuator and the heat conductor techniques were developed to remove geometry-related grain defects. In these techniques, the heat barrier that hinders lateral SC growth from the blade airfoil into the extremities of the platform is minimized. The parallel heating and cooling system was developed to achieve symmetric thermal conditions for SC solidification in blade clusters, thus considerably decreasing the negative shadow effect and its related defects in the current Bridgman process. The dipping and heaving technique, in which thinshell molds are utilized, was developed to enable the establishment of a high temperature gradient for SC growth and the freckle-free solidification of superalloy castings. Moreover, by applying the targeted cooling and heating technique, a novel concept for the three-dimensional and precise control of SC growth, a proper thermal arrangement may be dynamically established for the microscopic control of SC growth in the critical areas of large industrial gas turbine blades.

Solidification and crystal growth of solid solution semiconducting alloys

NASA Technical Reports Server (NTRS)

Lehoczky, S. L.; Szofran, F. R.

1984-01-01

Problems associated with the solidification and crytal growth of solid-solution semiconducting alloy crystals in a terrestrial environment are described. A detailed description is given of the results for the growth of mercury cadmium telluride (HgCdTe) alloy crystals by directional solidification, because of their considerable technological importance. A series of HgCdTe alloy crystals are grown from pseudobinary melts by a vertical Bridgman method using a wide range of growth rates and thermal conditions. Precision measurements are performed to establish compositional profiles for the crystals. The compositional variations are related to compositional variations in the melts that can result from two-dimensional diffusion or density gradient driven flow effects ahead of the growth interface. These effects are discussed in terms of the alloy phase equilibrium properties, the recent high temperature thermophysical data for the alloys and the highly unusual heat transfer characteristics of the alloy/ampule/furnace system that may readily lead to double diffusive convective flows in a gravitational environment.

Strategies for the coupling of global and local crystal growth models

NASA Astrophysics Data System (ADS)

Derby, Jeffrey J.; Lun, Lisa; Yeckel, Andrew

2007-05-01

The modular coupling of existing numerical codes to model crystal growth processes will provide for maximum effectiveness, capability, and flexibility. However, significant challenges are posed to make these coupled models mathematically self-consistent and algorithmically robust. This paper presents sample results from a coupling of the CrysVUn code, used here to compute furnace-scale heat transfer, and Cats2D, used to calculate melt fluid dynamics and phase-change phenomena, to form a global model for a Bridgman crystal growth system. However, the strategy used to implement the CrysVUn-Cats2D coupling is unreliable and inefficient. The implementation of under-relaxation within a block Gauss-Seidel iteration is shown to be ineffective for improving the coupling performance in a model one-dimensional problem representative of a melt crystal growth model. Ideas to overcome current convergence limitations using approximations to a full Newton iteration method are discussed.

Effects of doping impurity and growth orientation on dislocation generation in GaAs crystals grown from the melt: A qualitative finite-element study

NASA Astrophysics Data System (ADS)

Zhu, X. A.; Tsai, C. T.

2000-09-01

Dislocations in gallium arsenide (GaAs) crystals are generated by excessive thermal stresses induced during the crystal growth process. The presence of dislocations has adverse effects on the performance and reliability of the GaAs-based devices. It is well known that dislocation density can be significantly reduced by doping impurity atoms into a GaAs crystal during its growth process. A viscoplastic constitutive equation that couples the microscopic dislocation density with the macroscopic plastic deformation is employed in a crystallographic finite element model for calculating the dislocation density generated in the GaAs crystal during its growth process. The dislocation density is considered as an internal state variable and the drag stress caused by doping impurity is included in this constitutive equation. A GaAs crystal grown by the vertical Bridgman process is adopted as an example to study the influences of doping impurity and growth orientation on dislocation generation. The calculated results show that doping impurity can significantly reduce the dislocation density generated in the crystal. The level of reduction is also influenced by the growth orientation during the crystal growth process.

A comparison of point defects in Cd1-xZnxTe1-ySey crystals grown by Bridgman and traveling heater methods

NASA Astrophysics Data System (ADS)

Gul, R.; Roy, U. N.; Camarda, G. S.; Hossain, A.; Yang, G.; Vanier, P.; Lordi, V.; Varley, J.; James, R. B.

2017-03-01

In this paper, the properties of point defects in Cd1-xZnxTe1-ySey (CZTS) radiation detectors are characterized using deep-level transient spectroscopy and compared between materials grown using two different methods, the Bridgman method and the traveling heater method. The nature of the traps was analyzed in terms of their capture cross-sections and trap concentrations, as well as their effects on the measured charge-carrier trapping and de-trapping times, and then compared for the two growth techniques. The results revealed that Se addition to CdZnTe can reduce the VCd- concentration. In Travelling Heater Method (THM) and Bridgman Method (BM) grown CZTS detectors, besides a few similarities in the shallow and medium energy traps, there were major differences in the deep traps. It was observed that the excess-Te and lower growth-temperature conditions in THM-grown CZTS led to a complete compensation of VCd- and two additional traps (attributed to Tei- and TeCd++ appearing at around Ev + 0.26 eV and Ec - 0.78 eV, respectively). The 1.1-eV deep trap related to large Te secondary phases was a dominant trap in the BM-grown CZTS crystals. In addition to i-DLTS data, the effects of point defects induced due to different processing techniques on the detector's resistivity, spectral response to gammas, and μτ product were determined.

A Successful Synthesis of the CoCrFeNiAl0.3 Single-Crystal, High-Entropy Alloy by Bridgman Solidification

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

Ma, S. G.; Zhang, S. F.; Gao, M. C.

2013-08-22

For the first time, a face-centered-cubic, single-crystal CoCrFeNiAl{sub 0.3} (designated as Al0.3), high-entropy alloy (HEA) was successfully synthesized by the Bridgman solidification (BS) method, at an extremely low withdrawal velocity through a constant temperature gradient, for which it underwent two BS steps. Specially, at the first BS step, the alloy sample underwent several morphological transitions accompanying the crystal growth from the melt. This microstructure evolves from as-cast dendrites, to equiaxed grains, and then to columnar crystals, and last to the single crystal. In particular, at the equiaxed-grain region, some visible annealing twins were observed, which indicates a low stacking faultmore » energy of the Al0.3 alloy. Although a body-centered- cubic CoCrFeNiAl (Al1) HEA was also prepared under the same conditions, only a single columnar-crystal structure with instinctively preferential crystallographic orientations was obtained by the same procedure. A similar morphological transition from dendrites to equiaxed grains occurred at the equiaxed-grain region in Al1 alloy, but the annealing twins were not observed probably because a higher Al addition leads to a higher stacking fault energy for this alloy.« less

Vibroconvective mixing applied to vertical Bridgman growth

NASA Astrophysics Data System (ADS)

Zawilski, Kevin T.; Claudia, M.; Custodio, C.; DeMattei, Robert C.; Feigelson, Robert S.

2003-10-01

A promising method for stirring melts during vertical Bridgman growth is the coupled vibrational stirring (CVS) method. It involves the application of low frequency vibrations to the outside of the growth ampoule and produces strong flows emanating from the fluid surface. Although the technique was pioneered a number of years ago, previous studies have not provided sufficient information to explain how to control CVS generated flows in a particular system. This paper examines both the fluid flow produced by CVS and the effect of these flows on a model oxide growth system. CVS generated flows were studied using tracer particles in a water/glycerin system. The particle velocities were measured as a function of distance from the fluid surface. A large velocity gradient, decreasing from the surface, was found to be present. The velocity profile produced was dependent on the vibrational amplitude and frequency, the crucible diameter, and the fluid viscosity. The effects of CVS flows on the crystal growth interface were studied using NaNO 3 as a model oxide. Under non-growth conditions (i.e. no furnace or crucible translation), the solid-liquid interface position was found to be a strong function of vibrational frequency once CVS generated flows approached the interface. During crystal growth, undesirable growth rate fluctuations were found as the growth interface moved into regions of increasing fluid flow. This data suggests that a control system in which CVS flows are continuously decreased during growth to maintain a constant flow rate in the vicinity of the growth interface is necessary in order to prevent or reduce growth rate fluctuations.

Temperature and melt solid interface control during crystal growth

NASA Technical Reports Server (NTRS)

Batur, Celal

1990-01-01

Findings on the adaptive control of a transparent Bridgman crystal growth furnace are summarized. The task of the process controller is to establish a user specified axial temperature profile by controlling the temperatures in eight heating zones. The furnace controller is built around a computer. Adaptive PID (Proportional Integral Derivative) and Pole Placement control algorithms are applied. The need for adaptive controller stems from the fact that the zone dynamics changes with respect to time. The controller was tested extensively on the Lead Bromide crystal growth. Several different temperature profiles and ampoule's translational rates are tried. The feasibility of solid liquid interface quantification by image processing was determined. The interface is observed by a color video camera and the image data file is processed to determine if the interface is flat, convex or concave.

The composition effect on the thermal and optical properties across CdZnTe crystals

NASA Astrophysics Data System (ADS)

Strzałkowski, K.

2016-11-01

Cd1-x Zn x Te mixed crystals investigated in this work were grown from the melt using the vertical Bridgman-Stockbarger method in the whole range of composition 0  <  x  <  1 that is from one binary crystal (CdTe) to another (ZnTe). The real composition of grown crystals was measured with the SEM/EDS method along the growth axis. The segregation coefficient of Zn in a CdTe matrix has been evaluated as being close to unity. The energy gap as a function of the composition was determined from transmission spectroscopy. Thanks to that, the bowing parameter of this ternary alloy was found to be 0.458. In this work the systematical study of thermal properties of Cd1-x Zn x Te alloys from one binary crystal (CdTe) to another (ZnTe) grown by the vertical Bridgman technique were undertaken for the first time. The thermal diffusivity and effusivity of the investigated crystals were derived from the experimental data and allowed the thermal conductivity to be calculated. Diagrams of the thermal conductivity versus composition were analyzed applying the model for mixed semiconducting crystals given by Sadao Adachi. Thanks to that, the contribution of the thermal resistivity arising from the lattice disorder to the total resistivity of the crystal has been determined.

Thermal Modeling of Bridgman Crystal Growth

NASA Technical Reports Server (NTRS)

Cothran, E.

1983-01-01

Heat Flow modeled for moving or stationary rod shaped sample inside directional-solidification furnace. Program effectively models one-dimensional heat flow in translating or motionless rod-shaped sample inside of directionalsolidification furnace in which adiabatic zone separates hot zone and cold zone. Applicable to systems for which Biot numbers in hot and cold zones are less than unity.

Nonlinear Optical Phenomena in Solids

DTIC Science & Technology

1981-02-01

December 1980, organized according to research objectives: a. Objective: Grow five crystals of Hg].Cdx.Te by the modified Bridgman (quench/anneal) method...objectives of the contract are listed below: a. Grow five 2rystals of Hgl _ ,Cd T e by the modified Bridgman (quench/anneal) method. b. Determine the...composicinn and purity profiles of the crystals . c. Prepare spin-flip Raman laser cavities from selected sections of the crystals . d. Evaluate the utility of

Depth-Resolved Cathodoluminescence Study of Annealed Silicon Implanted Gallium Arsenide.

DTIC Science & Technology

1982-12-01

samples were Cr doped semi-insulat- ing GaAs crystals grown using the horizontal Bridgman method. Nine samples were prepared for this study, four were...function of depth. Cathodoluminescence was the excitation method. The crystals studied were grown using the horizontal Bridgman method. Four samples were...achieved by taking spectral data and successively chemically etching the surface of the crystal in 250 R steps. No new peaks were observed in the

Low Temperature Photoluminescence Characterization of Orbitally Grown CdZnTe

NASA Technical Reports Server (NTRS)

Ritter, Timothy M.; Larson, D. J.

1998-01-01

The II-VI ternary alloy CdZnTe is a technologically important material because of its use as a lattice matched substrate for HgCdTe based devices. The increasingly stringent requirements on performance that must be met by such large area infrared detectors also necessitates a higher quality substrate. Such substrate material is typically grown using the Bridgman technique. Due to the nature of bulk semiconductor growth, gravitationally dependent phenomena can adversely affect crystalline quality. The most direct way to alleviate this problem is by crystal growth in a reduced gravity environment. Since it requires hours, even days, to grow a high quality crystal, an orbiting space shuttle or space station provides a superb platform on which to conduct such research. For well over ten years NASA has been studying the effects of microgravity semiconductor crystal growth. This paper reports the results of photoluminescence characterization performed on an arbitrary grown CdZnTe bulk crystal.

An analytical approach to thermal modeling of Bridgman-type crystal growth. I - One-dimensional analysis

NASA Technical Reports Server (NTRS)

Naumann, R. J.

1982-01-01

A relatively simple one-dimensional thermal model of the Bridgman growth process has been developed which is applicable to the growth of small diameter samples with conductivities similar to those of metallic alloys. The heat flow in a translating rod is analyzed in a way that is applicable to Biot numbers less than unity. The model accommodates an adiabatic zone, different heat transfer coefficients in the hot and cold zones, and changes in sample material properties associated with phase change. The analysis is applied to several simplified cases. The effect of the rod's motion is studied in a three-zone furnace for a rod sufficiently long that end effects can be neglected; end effects are then investigated for a motionless rod. Finally, the addition of a fourth zone, an independently controlled booster heater between the main heater and the adiabatic zone, is evaluated for its ability to increase the gradient in the sample at the melt interface and to control the position of the interface.

Convective Flow Induced by Localized Traveling Magnetic Fields

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Rose, M. Franklin (Technical Monitor)

2001-01-01

An axisymmetric traveling magnetic field induces a meridional base flow in a cylindrical zone of an electrically conducting liquid. This remotely induced flow can be conveniently controlled, in magnitude and direction, and can have benefits for crystal growth applications. In particular, it can be used to offset natural convection. For long vertical cylinders, non-uniform and localized in the propagating direction, magnetic fields are required for this purpose. Here we investigate a particular form of this field, namely that induced by a set of a few electric current coils. An order of magnitude reduction of buoyancy convection is theoretically demonstrated for a vertical Bridgman crystal growth configuration.

A Comparison of Point Defects in Cd 1-xZn xTe 1-ySe y Crystals Grown by Bridgman and Traveling Heater Methods

DOE PAGES

Gul, R.; Roy, U. N.; Camarda, G. S.; ...

2017-03-28

In this study, the properties of point defects in Cd 1–xZn xTe 1–ySe y (CZTS) radiation detectors are characterized using deep-level transient spectroscopy and compared between materials grown using two different methods, the Bridgman method and the traveling heater method. The nature of the traps was analyzed in terms of their capture cross-sections and trap concentrations, as well as their effects on the measured charge-carrier trapping and de-trapping times, and then compared for the two growth techniques. The results revealed that Se addition to CdZnTe can reduce the V Cd – concentration. In Travelling Heater Method (THM) and Bridgman Methodmore » (BM) grown CZTS detectors, besides a few similarities in the shallow and medium energy traps, there were major differences in the deep traps. It was observed that the excess-Te and lower growth-temperature conditions in THM-grown CZTS led to a complete compensation of V Cd – and two additional traps (attributed to Te i – and Te Cd ++ appearing at around E v + 0.26 eV and E c – 0.78 eV, respectively). The 1.1-eV deep trap related to large Te secondary phases was a dominant trap in the BM-grown CZTS crystals. In addition to i-DLTS data, the effects of point defects induced due to different processing techniques on the detector's resistivity, spectral response to gammas, and μτ product were determined.« less

A Comparison of Point Defects in Cd 1-xZn xTe 1-ySe y Crystals Grown by Bridgman and Traveling Heater Methods

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

Gul, R.; Roy, U. N.; Camarda, G. S.

In this study, the properties of point defects in Cd 1–xZn xTe 1–ySe y (CZTS) radiation detectors are characterized using deep-level transient spectroscopy and compared between materials grown using two different methods, the Bridgman method and the traveling heater method. The nature of the traps was analyzed in terms of their capture cross-sections and trap concentrations, as well as their effects on the measured charge-carrier trapping and de-trapping times, and then compared for the two growth techniques. The results revealed that Se addition to CdZnTe can reduce the V Cd – concentration. In Travelling Heater Method (THM) and Bridgman Methodmore » (BM) grown CZTS detectors, besides a few similarities in the shallow and medium energy traps, there were major differences in the deep traps. It was observed that the excess-Te and lower growth-temperature conditions in THM-grown CZTS led to a complete compensation of V Cd – and two additional traps (attributed to Te i – and Te Cd ++ appearing at around E v + 0.26 eV and E c – 0.78 eV, respectively). The 1.1-eV deep trap related to large Te secondary phases was a dominant trap in the BM-grown CZTS crystals. In addition to i-DLTS data, the effects of point defects induced due to different processing techniques on the detector's resistivity, spectral response to gammas, and μτ product were determined.« less

Natural convection in melt crystal growth - The influence of flow pattern on solute segregation

NASA Technical Reports Server (NTRS)

Brown, R. A.; Yamaguchi, Y.; Chang, C. J.

1982-01-01

The results of two lines of research aimed at calculating the structure of the flows driven by buoyancy in small-scale crystal growth systems and at understanding the coupling between these flows, the shape of the solidification interface, and dopant segregation in the crystal are reviewed. First, finite-element methods are combined with computer-aided methods for detecting multiple steady solutions to analyze the structure of the buoyancy-driven axisymmetric flows in a vertical cylinder heated from below. This system exhibits onset of convection, multiple steady flows, and loss of the primary stable flow beyond a critical value of the Rayleigh number. Second, results are presented for calculations of convection, melt/solid interface shape, and dopant segregation within a vertical ampoule with thermal boundary conditions that represent a prototype of the vertical Bridgman growth system.

Simulation, modeling, and crystal growth of Cd0.9Zn0.1Te for nuclear spectrometers

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Kang, Sung Hoon; Choi, Michael; Bello, Job; Zheng, Lili; Zhang, Hui; Groza, Michael; Roy, Utpal N.; Burger, Arnold; Jellison, Gerald E.; Holcomb, David E.; Wright, Gomez W.; Williams, Joseph A.

2006-06-01

High-quality, large (10 cm long and 2.5 cm diameter), nuclear spectrometer grade Cd0.9Zn0.1Te (CZT) single crystals have been grown by a controlled vertical Bridgman technique using in-house zone refined precursor materials (Cd, Zn, and Te). A state-of-the-art computer model, multizone adaptive scheme for transport and phase-change processes (MASTRAP), is used to model heat and mass transfer in the Bridgman growth system and to predict the stress distribution in the as-grown CZT crystal and optimize the thermal profile. The model accounts for heat transfer in the multiphase system, convection in the melt, and interface dynamics. The grown semi-insulating (SI) CZT crystals have demonstrated promising results for high-resolution room-temperature radiation detectors due to their high dark resistivity (ρ≈2.8 × 1011 Θ cm), good charge-transport properties [electron and hole mobility-life-time product, μτe≈(2 5)×10-3 and μτh≈(3 5)×10-5 respectively, and low cost of production. Spectroscopic ellipsometry and optical transmission measurements were carried out on the grown CZT crystals using two-modulator generalized ellipsometry (2-MGE). The refractive index n and extinction coefficient k were determined by mathematically eliminating the ˜3-nm surface roughness layer. Nuclear detection measurements on the single-element CZT detectors with 241Am and 137Cs clearly detected 59.6 and 662 keV energies with energy resolution (FWHM) of 2.4 keV (4.0%) and 9.2 keV (1.4%), respectively.

Multidisciplinary Approaches to Radiation Balanced Lasers (MARBLe): 1st Annual Progress Report

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

Hehlen, Markus Peter

The initial main modifications of the existing μPD crystal-growth system at LANL have been completed. This now gives us the new capability to develop the growth of crystalline RBL materials by both the μPD and the Bridgman method. Quantitative mass spectrometry of the growth atmosphere was conducted to identify possible sources of gaseous trace species (primarily hydrogen) that could cause the undesired reduction of Yb 3+ to Yb 2+ during the crystal growth. Hydrogen was found to be at sufficiently low levels to not be a respective concern. Studies on the thermal decomposition of YbF 3 to form Yb 2+more » are currently underway in collaboration with MARBLe team member Prof. Pauzauskie. First samples of Yb 3+-doped YLiF 4 (YLF:Yb) and undoped LiLuF 4 (LLF) were grown, and MARBLe team member Prof. Sheik-Bahae has performed measurements of laser-induced heating (YLF:Yb) and background absorption coefficient (LLF). We discovered that one or several of the YF 3, LiF, and YbF 3 precursors contains organic impurities that chemically reduce to black residue during the high-temperature growth in oxygen-free argon atmosphere. A process for removal of these residues prior to growth is being considered. Comparing the results from incongruently melting YLF with those of congruently melting LLF indicate that a congruently melting material is preferred for Bridgman growth. Crystal-growth experiments with LLF are currently underway. The results of these studies on Yb 3+ doped materials will be directly applicable to the future growth of Er 3+ and Tm 3+ doped as well as Yb 3+, Nd 3+ co-doped RBL crystals. There was no activity on the parallel effort of developing rareearth- doped chalcogenide glasses. The primary reason was a lack of manpower due to a delayed hiring of a student. In September 2017, we have hired a Postdoctoral Researcher who will be able to contribute to the growth (at LANL) and optical characterization (at UNM) of RBL materials.« less

Growth of InSb and InI Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Churilov, A.; Volz, M. P.; Riabov, V.; Van den Berg, L.

2015-01-01

During the past 40 years, dozens of semiconductor crystal growth experiments have been conducted in space laboratories. The subsequent analysis of the space-grown crystals revealed (i) that weak convection existed in virtually all melt-growth experiments, (ii) de-wetting significantly reduced the level of stress-induced defects, and (iii) particularly encouraging results were obtained in vapor-growth experiments. In 2002, following a decade of ground based research in growing doped Ge and GaSb crystals, a series of crystal growth experiments was performed at the ISS, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation. Te- and Zn-doped InSb crystals were grown from the melt. The specially designed furnace provided a side-view of the melt and precise seeding measurement of the growth rate. At present, under sponsorship of CASIS (Center for the Advancement of Science in Space, www.iss-casis.org), we are conducting ground-based experiments with indium mono-iodide (InI) in preparation for the "SUBSA II" ISS investigation, planned for 2017. The experiments include: i) Horizontal Bridgman (HB) growth and ii) Vapor Transport (VT) growth. Finite element modeling will also be conducted, to optimize the design of the flight ampoules, for vapor and melt growth.

Growth and properties of benzil doped benzimidazole (BMZ) single crystals

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

Babu, R. Ramesh, E-mail: rampap2k@yahoo.co.in; Crystal Growth and Crystallography Section, National Physical Laboratory, Krishnan Marg, New Delhi 110 012; Sukumar, M.

2010-09-15

In the present work, we have made an attempt to study the effect of benzil doping on the properties of benzimidazole single crystals. For this purpose we have grown pure and benzil doped benzimidazole single crystals by vertical Bridgman technique. The grown crystals were characterized by various characterization techniques. The presence of dopants confirmed by powder X-ray diffraction (XRD). Crystalline perfection of the grown crystals has been analysed by high-resolution X-ray diffraction (HRXRD). The transmittance, electrical property and mechanical strength have been analysed using UV-vis-NIR spectroscopic, dielectric and Vicker's hardness studies. The relative second harmonic generation efficiency of pure andmore » doped benzimidazole crystals measured using Kurtz powder test.« less

Fluorescence Properties of Fe2+- and Co2+-doped Hosts of CdMnTe Compositions as Potential Mid-Infrared Laser Materials

DTIC Science & Technology

2011-09-01

composition also affects the Co2+ and Fe2+ dopant lifetimes and temperature dependencies. Crystal growth effort is underway in order to improve the...single-crystalline samples of Fe2+ or divalent cobalt ion (Co2+)-doped CMT crystals were produced by Brimrose Corporation using a modified vertical...Bridgman technique (18). The starting high purity ingredients Cd, Mn, and Te along with the dopants (Fe and Co) are placed in a pre-cleaned and baked

Effect of Elevated Pressure on the Heat Transfer and Power Requirements During Bridgman Growth of PMN-PT Crystals

NASA Technical Reports Server (NTRS)

Bune, Andris; Ostrogorsky, Aleksandar; Marin, Carlos; Nicoara, Irina; Rose, M. Franklin (Technical Monitor)

2000-01-01

Performance of the furnace during Bridgman growth of the lead magnesium niobate-lead titanate crystal (PMN-PT) is analyzed. PMN-PT is electrostrictive ceramic that has near ideal strain-voltage function. Furthermore piezoelectric (2000 to 2300 pC/N) and coupling (92 to 95%) constants are exceptionally good. Due to these properties PMN-PT has wide range of applications - from sonars to transducers in a high precision optical systems. In this research first attempt to crystallize PMN-PT in a Mellen type vertical Bridgman furnace was not successful, as melting temperature of precursor materials was not achieved. At this point choice was between building a new more powerful facility or finding ways to enhance performance of the existing furnace. Besides adjusting power supply to the individual heating elements, redesigning ampoule holding cartridge and improving furnace insulation one more radical improvement was proposed. The entire furnace was placed into the high pressure chamber. Further experiments confirmed that temperature inside the furnace was increased sufficiently to melt precursor materials to obtain PMN-PT. Numerical modeling is undertaken to find limitations of this technique and to predict temperature distribution inside the ampoule. It is of interest also to account for main factors contributing to a higher temperatures achieved in the furnace under the higher pressure (up to 10 atm.). Numerical model of the furnace is based on general purpose finite - element code FIDAP and on previous efforts to model Bridgman type furnace with multiply heaters. In order to account for all heat transfer mechanism involved - conduction, convection and radiation - different parts of the furnace are modeled in accordance with expected dominant mode of heat transfer - conduction in the solid parts, conduction and radiation in the ampoule, gas convection and conduction in the furnace openings complemented with wall-to-wall radiation. Because of these complicating factors, dimensional rather than non-dimensional modeling is performed using steady-state 2-D and 3-D models. Particular attention is paid to the modeling of radiation in a semitransparent material of ampoule 7 sapphire. The radiation model is validated by solving realistic test problem - conduction and radiation heat transfer in the fused quartz. Results are in agreement with both experimental and analytical data.

Organic/inorganic-doped aromatic derivative crystals: Growth and properties

NASA Astrophysics Data System (ADS)

Stanculescu, F.; Ionita, I.; Stanculescu, A.

2014-09-01

Results of a comparative study on the growth from melt by the Bridgman-Stockbarger method of meta-dinitrobenzene (m-DNB) and benzil (Bz) crystals in the same experimental set-up and the same experimental conditions are presented. The incorporation of an inorganic (iodine) dopant in m-DNB was analyzed in the given experimental conditions from the point of view of the solid-liquid interface stability. The limits for a stable growth and the conditions that favor the generation of morphological instability are emphasized. These limits for m-DNB are compatible with those previously determined for Bz, and therefore, even for a high gradient concentration at the growth interface, it is possible to grow m-DNB and Bz crystals in the same experimental conditions characterized by a high ΔT and v. The optical properties were investigated in relation with the dopant incorporation in the crystal in the mentioned experimental conditions. Effects of the dopant (m-DNB/iodine in Bz and iodine in m-DNB) on the optical band gap and optical non-linear properties of the crystals are discussed.

Growth of 1.5-In Eu : SrI2 Single Crystal and Scintillation Properties

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Ito, Tomoki; Yasuhiro, Shoji; Kurosawa, Shunsuke; Ohashi, Yuji; Kamada, Kei; Yoshikawa, Akira

2016-04-01

We grew 1.5-in Eu doped SrI2 (Eu : SrI2) bulk single crystal by a modified vertical Bridgman (VB) method using a removable chamber and high-frequency induction heating. Asgrown 1.5-in Eu : SrI2 bulk single crystal had no visible crack and inclusion in the crystal. In the transmittance and α-ray radioluminescence spectra, large absorption below 433 nm and emission peak at 433 nm were observed, respectively. Each polished Eu : SrI2 specimen indicated 56 000 62 000 ph/MeV light yield and 3.3 3.9% energy resolution. The decay times of the specimens were 0.61 0.67 μs.

Large-size TlBr single crystal growth and defect study

NASA Astrophysics Data System (ADS)

Zhang, Mingzhi; Zheng, Zhiping; Chen, Zheng; Zhang, Sen; Luo, Wei; Fu, Qiuyun

2018-04-01

Thallium bromide (TlBr) is an attractive semiconductor material for fabrication of radiation detectors due to its high photon stopping power originating from its high atomic number, wide band gap and high resistivity. In this paper the vertical Bridgman method was used for crystal growth and TlBr single crystals with diameter of 15 mm were grown. X-ray diffraction (XRD) was used to identify phase and orientation. Electron backscatter diffraction (EBSD) was used to investigate crystal microstructure and crystallographic orientation. The optical and electric performance of the crystal was characterized by infrared (IR) transmittance spectra and I-V measurement. The types of point defects in the crystals were investigated by thermally stimulated current (TSC) spectra and positron annihilation spectroscopy (PAS). Four types of defects, with ionization energy of each defect fitting as follows: 0.1308, 0.1540, 0.3822 and 0.538 eV, were confirmed from the TSC result. The PAS result showed that there were Tl vacancies in the crystal.

Advanced methods for preparation and characterization of infrared detector materials. [mercury cadmium tellurides

NASA Technical Reports Server (NTRS)

Lehoczky, S. L.; Szofran, F. R.; Martin, B. G.

1980-01-01

Mercury cadmium telluride crystals were prepared by the Bridgman method with a wide range of crystal growth rates and temperature gradients adequate to prevent constitutional supercooling under diffusion-limited, steady state, growth conditions. The longitudinal compositional gradients for different growth conditions and alloy compositions were calculated and compared with experimental data to develop a quantitative model of the crystal growth kinetics for the Hg(i-x)CdxTe alloys, and measurements were performed to ascertain the effect of growth conditions on radial compositional gradients. The pseudobinary HgTe-CdTe constitutional phase diagram was determined by precision differential thermal analysis measurements and used to calculate the segregation coefficient of Cd as a function of x and interface temperature. Computer algorithms specific to Hg(1-x)CdxTe were developed for calculations of the charge carrier concentrations, charge carrier mobilities, Hall coefficient, optical absorptance, and Fermi energy as functions of x, temperature, ionized donor and acceptor concentrations, and neutral defect concentrations.

On the effect of thermodiffusion on solute segregation during the growth of semiconductor materials by the vertical Bridgman method

NASA Astrophysics Data System (ADS)

Ben Sassi, Mokhtar; Kaddeche, Slim; Lappa, Marcello; Millet, Séverine; Henry, Daniel; Ben Hadid, Hamda

2017-01-01

The effect of thermodiffusion on dopant distribution in the melt and in the grown crystal is investigated numerically for a vertical Bridgman configuration for situations of pure thermal convection corresponding to dilute alloys. The dopant distribution is shown to be significantly affected by the Soret parameter value. The sensitivity of the system to a variety of parameters, including the Grashof number and the so-called furnace residence time, i.e. the time during which the crucible is maintained in the furnace before initiating the solidification process, is assessed by means of parametric simulations. Moreover, the results indicate that variations in the sign of the Soret parameter can lead to diametrically opposite behaviors, while an increase in the intensity of the thermal convection generally leads to a mitigation of the effects induced by thermodiffusion. On the basis of the numerical results some useful criteria are drawn which could help crystal growers to discern the complex interrelations among the various parameters under one's control (that are not independent of one another) and to elaborate rational guidelines relating to strategies to be used to improve the quality of the resulting crystals.

Vertical Bridgman growth and characterization of Cd 0.95-xMn xZn 0.05Te (x=0.20, 0.30) single-crystal ingots

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

Bolotnikov, A.; Kopach, V.; Kopach, O.

Solid-liquid phase transitions in Cd 0.95-xMn xZn 0.05Te alloys with x = 0.20 and 0.30 were investigated by differential thermal analysis (DTA). The heating/cooling rates were 5 and 10 K/min with a melt dwell time of 10, 30 and 60 minutes. Cd 0.95-xMn xZn 0.05Te (x=0.20, 0.30) single-crystal ingots were grown by the vertical Bridgman method guided using the DTA results. Te inclusions (1-20 microns), typical for CdTe and Cd(Zn)Te crystals, were observed in the ingots by infrared transmission microscopy. The measured X-ray diffraction patterns showed that all compositions are found to be in a single phase. Using current-voltage (I-V)more » measurements, the resistivity of the samples from each ingot was estimated to be about 10 5 Ohm·cm. The optical transmission analysis demonstrated that the band-gap width of the investigated ingots increased from 1.77 to 1.88 eV with the increase of the MnTe content from 20 to 30 mol. %.« less

Growth, spectroscopy and continuous-wave laser performance of Nd3+:LiLu0.65Y0.35F4 crystal

NASA Astrophysics Data System (ADS)

Demesh, M. P.; Kurilchik, S. V.; Gusakova, N. V.; Yasukevich, A. S.; Kisel, V. E.; Nizamutdinov, A. S.; Marisov, M. M.; Aglyamov, R. D.; Korableva, S. L.; Naumov, A. K.; Semashko, V. V.; Kuleshov, N. V.

2018-04-01

A mixed fluoride crystal of LiLu0.65Y0.35F4 doped with Nd3+ ions was grown by the Bridgman-Stockbarger method. Polarized absorption and luminescence spectra as well as luminescence lifetime were measured at room temperature. Emission probabilities, branching ratios and radiative lifetime were studied within the Judd-Ofelt theory and the emission cross section spectra were calculated. Efficient continuous wave laser operation was demonstrated with the crystal. A maximum output power of 7.7 W and slope efficiency of 60% were achieved at 1047 nm for the TEM00 mode.

Growth Angle - a Microscopic View

NASA Technical Reports Server (NTRS)

Mazurak, K.; Volz, M. P.; Croll, A.

2017-01-01

The growth angle that is formed between the side of the growing crystal and the melt meniscus is an important parameter in the detached Bridgman crystal growth method, where it determines the extent of the crystal-crucible wall gap, and in the Czochralski and float zone methods, where it influences the size and stability of the crystals. The growth angle is a non-equilibrium parameter, defined for the crystal growth process only. For a melt-crystal interface translating towards the crystal (melting), there is no specific angle defined between the melt and the sidewall of the solid. In this case, the corner at the triple line becomes rounded, and the angle between the sidewall and the incipience of meniscus can take a number of values, depending on the position of the triple line. In this work, a microscopic model is developed in which the fluid interacts with the solid surface through long range van der Waals or Casimir dispersive forces. This growth angle model is applied to Si and Ge and compared with the macroscopic approach of Herring. In the limit of a rounded corner with a large radius of curvature, the wetting of the melt on the crystal is defined by the contact angle. The proposed microscopic approach addresses the interesting issue of the transition from a contact angle to a growth angle as the radius of curvature decreases.

Oxygen in GaAs - Direct and indirect effects

NASA Technical Reports Server (NTRS)

Gatos, H. C.; Skowronski, M.; Pawlowicz, L.; Lagowski, J.

1984-01-01

Oxygen has profound effects on the key electronic properties and point defects of GaAs crystals. Thus, when added in the growth system, it decreases the free electron concentration and enhances the concentration of deep donors in the resulting crystals. Both of these effects are highly beneficial for achieving semi-insulating material and have been utilized for that purpose. They have been attributed to the tendency of oxygen to getter silicon impurities during crystal growth. Only recently, it has been found that oxygen in GaAs introduces also a midgap level, ELO, with essentially the same activation energy as EL2 but with four times greater electron capture cross section. The present report reassesses the electrical and optical properties of the midgap levels in GaAs crystals grown by the horizontal Bridgman (HB) and the Czochralski-LEC techniques. Emphasis is placed on the identification of the specific effects of ELO.

Features of bicrystal growth during the directional crystallization of metal melts

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

Gubernatorov, V. V.; Sycheva, T. S., E-mail: sych@imp.uran.ru; Gundyrev, V. M.

2017-03-15

The factors responsible for the formation of different configurations of boundaries between adjacent crystallites during their growth from melt by Bridgman and Czochralski methods have been considered by an of example Fe–20 wt % Ga alloy and Ni bicrystals. It is found that the configuration of intercrystallite boundary is related to the features of crystallite growth, caused by the strained state of intercrystallite and interphase (crystal–melt) boundaries, the difference in the linear thermal expansion coefficients of the crystallite boundaries and bulk, and the shape (geometry) of the bicrystal cross section. It is suggested that the strained state of boundaries andmore » the formation of substructure in crystallites during directional crystallization from metal melt are significantly affected by their deformation under the melt weight.« less

Growth of 2 Inch Eu-doped SrI2 single crystals for scintillator applications

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Shoji, Yasuhiro; Yokota, Yuui; Kurosawa, Shunsuke; Hayasaka, Shoki; Chani, Valery I.; Ito, Tomoki; Kamada, Kei; Ohashi, Yuji; Kochurikhin, Vladimir

2016-10-01

A vertical Bridgman (VB) crystal growth process was established using modified micro-pulling-down (μ-PD) crystal growth system with a removable chamber that was developed for the growth of deliquescent halide single crystals because conventional μ-PD method does not allow growth of large bulk single crystals. Eu:SrI2 crystals were grown from the melt of (Sr0.98Eu0.02)I2 composition using carbon crucibles. Undoped μ-PD SrI2 crystals were used as seeds that were affixed to the bottom of the crucible. All the preparations preceding the growths and the hot zone assembling were performed in a glove box with Ar gas. Then the removable chamber was taken out of the glove box, attached to the μ-PD system, connected with a Turbo Molecular pump, and evacuated down to 10-4 Pa at 300 °C. After the baking procedure, high purity Ar gas (6N) was injected into the chamber. The crucible was heated by a high frequency induction coil up to the melting point of Eu:SrI2. After melting the starting materials, the crucible was displaced in downward direction for the crystal growth and then cooled down to room temperature. Thus, 2 in. and crack-free Eu:SrI2 bulk crystals were produced. The crystals had high transparency and did not contain any visible inclusions. The crystals were cut and polished in the glove box and then sealed in an aluminum container with an optical window for characterization. The details of the crystal growth are discussed.

Amplitudes of doping striations: comparison of numerical calculations and analytical approaches

NASA Astrophysics Data System (ADS)

Jung, T.; Müller, G.

1997-02-01

Transient, axisymmetric numerical calculations of the heat and species transport including convection were performed for a simplified vertical gradient freeze (Bridgman) process with bottom seeding for GaAs. Periodical oscillations were superimposed onto the transient heater temperature profile. The amplitudes of the resulting oscillations of the growth rate and the dopant concentration (striations) in the growing crystals are compared with the predictions of analytical models.

Combined distillation and normal freezing to purify elements of groups II and VI

NASA Technical Reports Server (NTRS)

Holland, L. R.

1984-01-01

A practical system and its application to the purification of Te and Cd is described. Single crystals are grown directly in vitreous silica ampoules subsequently used for sealed Bridgman growth of (Hg-Cd)Te. The system also prepares the ampoules by heating in high vacuum. Purification of the elements is by the combined effect of distillation and normal freezing. Transport and segregation are discussed.

Dewetting During the Crystal Growth of (Cd,Zn)Te:In Under Microgravity

NASA Astrophysics Data System (ADS)

Sylla, Lamine; Fauler, Alex; Fiederle, Michael; Duffar, Thierry; Dieguez, Ernesto; Zanotti, Lucio; Zappettini, Andrea; Roosen, GÉrald

2009-08-01

The phenomenon of ldquodewettingrdquo associated with the Vertical Bridgman (VB) crystal growth technique leads to the growth of a crystal without contact with the crucible. One dramatic consequence of this modified VB process is the reduction of structural defects within the crystal. It has been observed in several microgravity experiments for different semiconductor crystals. This work is concentrated on the growth of high resistivity (Cd,Zn)Te:In (CZT) crystals by achieving the phenomenon of dewetting under microgravity condition and its application in the processing of CZT detectors. Two Cd0.9Zn0.1Te:In crystals were grown in space on the Russian FOTON satellite in the POLIZON-M facility in September 2007 (mission M3). At the end of the preliminary melting phase of one crystal, a Rotating Magnetic Field (RMF) was applied in order to reduce the typical tellurium clusters within the melt before the pulling. The other crystal was superheated with 20 K above the melting point before the pulling. A third reference crystal has been grown on the ground in similar thermal conditions. Profiles measurements of the space grown crystals surface gave the evidence of a successful dewetting during the crystal growth. Characterization methods such as IR microscopy and CoReMa have been performed on the three crystals. CZT detectors have been processed from the grown part of the different crystals. The influence of the dewetting on the material quality and the detector properties completes the study.

Process modelling for materials preparation experiments

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Alexander, J. Iwan D.

1993-01-01

The main goals of the research under this grant consist of the development of mathematical tools and measurement of transport properties necessary for high fidelity modeling of crystal growth from the melt and solution, in particular, for the Bridgman-Stockbarger growth of mercury cadmium telluride (MCT) and the solution growth of triglycine sulphate (TGS). Of the tasks described in detail in the original proposal, two remain to be worked on: (1) development of a spectral code for moving boundary problems; and (2) diffusivity measurements on concentrated and supersaturated TGS solutions. Progress made during this seventh half-year period is reported.

Process modelling for materials preparation experiments

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Alexander, J. Iwan D.

1993-01-01

The main goals of the research consist of the development of mathematical tools and measurement of transport properties necessary for high fidelity modeling of crystal growth from the melt and solution, in particular for the Bridgman-Stockbarger growth of mercury cadmium telluride (MCT) and the solution growth of triglycine sulphate (TGS). Of the tasks described in detail in the original proposal, two remain to be worked on: development of a spectral code for moving boundary problems, and diffusivity measurements on concentrated and supersaturated TGS solutions. During this eighth half-year period, good progress was made on these tasks.

Process modelling for materials preparation experiments

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Alexander, J. Iwan D.

1992-01-01

The development is examined of mathematical tools and measurement of transport properties necessary for high fidelity modeling of crystal growth from the melt and solution, in particular for the Bridgman-Stockbarger growth of mercury cadmium telluride (MCT) and the solution growth of triglycine sulphate (TGS). The tasks include development of a spectral code for moving boundary problems, kinematic viscosity measurements on liquid MCT at temperatures close to the melting point, and diffusivity measurements on concentrated and supersaturated TGS solutions. A detailed description is given of the work performed for these tasks, together with a summary of the resulting publications and presentations.

Synthesis of a potential semiconductor neutron detector crystal LiGa(Se/Te)2: materials purity and compatibility effects

NASA Astrophysics Data System (ADS)

Stowe, Ashley C.; Morrell, J.; Battacharya, Pijush; Tupitsyn, Eugene; Burger, Arnold

2011-09-01

Lithium containing AIBIIICVI semiconductors are being considered as alternative materials for room temperature neutron detection. One of the primary challenges in growing a high quality crystal of such a material is the reactivity of lithium metal. The presence of nitrides, oxides, and a variety of alkali and alkaline earth metal impurities prevent pure synthesis and truncate crystal growth by introducing multiple nucleation centers during growth. Multiple lithium metal purification methods have been investigated which ultimately raised the metal purity to 99.996%. Multi-cycle vacuum distillation removed all but 40 ppm of metal impurities in lithium metal. LiGa(Se/Te)2 was then synthesized with the high purity lithium metal by a variety of conditions. Lithium metal reacts violently with many standard crucible materials, and thermodynamic studies were undertaken to insure that an appropriate crucible choice was made, with high purity iron and boron nitride crucibles being the least reactive practical materials. Once conditions were optimized for synthesis of the chalcopyrite, vertical Bridgman crystal growth resulted in red crystals. The optical, electronic, and thermodynamic properties were collected.

Compositional homogeneity and X-ray topographic analyses of CdTe xSe 1-x grown by the vertical Bridgman technique

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-01

We grew CdTe xSe 1-x crystals with nominal Se concentrations of 5%, 7%, and 10% by the vertical Bridgman technique, and evaluated their compositional homogeneity and structural quality at the NSLS’ X-ray fluorescence and white beam X-ray topography beam lines. Both X-ray fluorescence and photoluminescence mapping revealed very high compositional homogeneity of the CdTe xSe 1-x crystals. Here, we noted that those crystals with higher concentrations of Se were more prone to twinning than those with a lower content. The crystals were fairly free from strains and contained low concentrations of sub-grain boundaries and their networks.

Crystal Growth and Scintillation Properties of Eu2+ doped Cs4CaI6 and Cs4SrI6

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Chakoumakos, B.; Johnson, J.; Loyd, M.; Wu, Y.; Koschan, M.; Melcher, C. L.

2018-03-01

In this work we present the crystal growth and scintillation properties of two new ternarymetal halide scintillators activated with divalent europium, Cs4CaI6 and Cs4SrI6. Single crystals of each compound were grown in evacuated quartz ampoules via the vertical Bridgman technique using a two-zone transparent furnace. Single crystal X-ray diffraction experiments showed that both crystals have a trigonal (R-3c) structure, with a density of 3.99 g/cm3 and 4.03 g/cm3. The radioluminescence and photoluminescence measurements showed typical luminescence properties due to the 5d-4f radiative transitions in Eu2+. At this early stage of development Cs4SrI6:Eu and Cs4CaI6:Eu have shown very promising scintillation properties, with light yields and energy resolutions of 62,300 ph/MeV and 3.3%, and 51,800 photons/MeV and 3.6% at 662 keV, respectively.

Optimal design of solidification processes

NASA Technical Reports Server (NTRS)

Dantzig, Jonathan A.; Tortorelli, Daniel A.

1991-01-01

An optimal design algorithm is presented for the analysis of general solidification processes, and is demonstrated for the growth of GaAs crystals in a Bridgman furnace. The system is optimal in the sense that the prespecified temperature distribution in the solidifying materials is obtained to maximize product quality. The optimization uses traditional numerical programming techniques which require the evaluation of cost and constraint functions and their sensitivities. The finite element method is incorporated to analyze the crystal solidification problem, evaluate the cost and constraint functions, and compute the sensitivities. These techniques are demonstrated in the crystal growth application by determining an optimal furnace wall temperature distribution to obtain the desired temperature profile in the crystal, and hence to maximize the crystal's quality. Several numerical optimization algorithms are studied to determine the proper convergence criteria, effective 1-D search strategies, appropriate forms of the cost and constraint functions, etc. In particular, we incorporate the conjugate gradient and quasi-Newton methods for unconstrained problems. The efficiency and effectiveness of each algorithm is presented in the example problem.

Modeling of convection phenomena in Bridgman-Stockbarger crystal growth

NASA Technical Reports Server (NTRS)

Carlson, F. M.; Eraslan, A. H.; Sheu, J. Z.

1985-01-01

Thermal convection phenomena in a vertically oriented Bridgman-Stockbarger apparatus were modeled by computer simulations for different gravity conditions, ranging from earth conditions to extremely low gravity, approximate space conditions. The modeling results were obtained by the application of a state-of-the art, transient, multi-dimensional, completely densimetrically coupled, discrete-element computational model which was specifically developed for the simulation of flow, temperature, and species concentration conditions in two-phase (solid-liquid) systems. The computational model was applied to the simulation of the flow and the thermal conditions associated with the convection phenomena in a modified Germanium-Silicon charge enclosed in a stationary fused-silica ampoule. The results clearly indicated that the gravitational field strength influences the characteristics of the coherent vortical flow patterns, interface shape and position, maximum melt velocity, and interfacial normal temperature gradient.

Magneto-Hydrodynamic Damping of Convection During Vertical Bridgman-Stockbarger Growth of HgCdTe

NASA Technical Reports Server (NTRS)

Watring, D. A.; Lehoczky, S. L.

1996-01-01

In order to quantify the effects of convection on segregation, Hg(0.8)Cd(0.2)Te crystals were grown by the vertical Bridgman-Stockbarger method in the presence of an applied axial magnetic field of 50 kG. The influence of convection, by magneto-hydrodynamic damping, on mass transfer in the melt and segregation at the solid-liquid interface was investigated by measuring the axial and radial compositional variations in the grown samples. The reduction of convective mixing in the melt through the application of the magnetic field is found to decrease radial segregation to the diffusion-limited regime. It was also found that the suppression of the convective cell near the solid-liquid interface results in an increase in the slope of the diffusion-controlled solute boundary layer, which can lead to constitutional supercooling.

The Influence of Low Frequency Mechanical Vibrations on the Growth of Single Crystals

NASA Technical Reports Server (NTRS)

Feigelson, R. S.; Elwell, D.

1985-01-01

The optimum conditions for crystal growth are usually achieved either by suppressing convective fluid flows (e.g., by the use of a low-gravity environment) or by over-riding thermal and solutal convection by the use of a strong stirring action. A novel stirring technique has been developed which involves subjecting a vertical crucible to a circle in a horizontal plane (without rotation). Use of an amplitude of 3 mm at a frequency of approx 6 Hz produced complete mixing of a non-uniform aqueous liquid in a few seconds. The mixing action involved the downward flow of liquid in the outer annulus of the liquid, driven by surface waves. When the downward flowing liquid reaches the bottom of the crucible, it is reflected in a central, upward flowing spiral. This flow pattern should be beneficial for crystal growth by the Bridgman method since it will sweep impurities away from the walls and produce a more convex solid-liquid interface. Initial attempts to apply the new stirring technique to CdTe crystal growth did not show significant improvement in the number of crystals nucleated, but the interface shape appeared to be close to that predicted.

High resolution synchrotron X-radiation diffraction imaging of crystals grown in microgravity and closely related terrestrial crystals

NASA Technical Reports Server (NTRS)

Steiner, Bruce; Dobbyn, Ronald C.; Black, David; Burdette, Harold; Kuriyama, Masao; Fripp, Archibald; Simchik, Richard

1991-01-01

Irregularities in three crystals grown in space and in four terrestrial crystals grown under otherwise comparable conditions have been observed in high resolution diffraction imaging. The images provide important new clues to the nature and origins of irregularities in each crystal. For two of the materials, mercuric iodide and lead tin telluride, more than one phase (an array of non-diffracting inclusions) was observed in terrestrial samples; but the formation of these multiple phases appears to have been suppressed in directly comparable crystals grown in microgravity. The terrestrial seed crystal of triglycine sulfate displayed an unexpected layered structure, which propagated during directly comparable space growth. Terrestrial Bridgman regrowth of gallium arsenide revealed a mesoscopic structure substantially different from that of the original Czochralski material. A directly comparable crystal is to be grown shortly in space.

Two-Step Vapor/Liquid/Solid Purification

NASA Technical Reports Server (NTRS)

Holland, L. R.

1986-01-01

Vertical distillation system combines in single operation advantages of multiple zone refining with those of distillation. Developed specifically to load Bridgman-Stockbarger (vertical-solidification) growth ampoules with ultrapure tellurium and cadmium, system, with suitable modifications, serves as material refiner. In first phase of purification process, ampoule heated to drive off absorbed volatiles. Second phase, evaporator heated to drive off volatiles in charge. Third phase, slowly descending heater causes distillation from evaporator to growing crystal in ampoule.

GaSe and GaTe anisotropic layered semiconductors for radiation detectors

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Choi, Michael; Kang, Sung Hoon; Rauh, R. David; Wei, Jiuan; Zhang, Hui; Zheng, Lili; Cui, Y.; Groza, M.; Burger, A.

2007-09-01

High quality detector grade GaSe and GaTe single crystals have been grown by a modified vertical Bridgman technique using high purity Ga (7N) and in-house zone refined (ZR) precursor materials (Se and Te). A state-of-the-art computer model, MASTRAPP, is used to model heat and mass transfer in the Bridgman growth system and to predict the stress distribution in the as-grown crystals. The model accounts for heat transfer in the multiphase system, convection in the melt, and interface dynamics. The crystals harvested from ingots of 8-10 cm length and 2.5 cm diameter, have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, low temperature photoluminescence (PL), atomic force microscopy (AFM), and optical absorption/transmission measurements. Single element devices up to 1 cm2 in area have been fabricated from the crystals and tested as radiation detectors by measuring current-voltage (I-V) characteristics and pulse height spectra using 241Am source. The crystals have shown high promise as nuclear detectors with their high dark resistivity (>=10 9 Ω .cm), good charge transport properties (μτ e ~ 1.4x10 -5 cm2/V and μτ h ~ 1.5x10 -5 cm2/V), and relatively good energy resolution (~4% energy resolution at 60 keV). Details of numerical modeling and simulation, detector fabrication, and testing using a 241Am energy source (60 keV) is presented in this paper.

On the Role of Boron in CdTe and CdZnTe Crystals

NASA Astrophysics Data System (ADS)

Pavesi, M.; Marchini, L.; Zha, M.; Zappettini, A.; Zanichelli, M.; Manfredi, M.

2011-10-01

It is well known that group III elements act as donors if they play a substitutional role at the metallic site in II-tellurides; nevertheless, several studies report both on the creation of complexes with vacancies, named A-centers, and on the involvement in self-compensation mechanisms, especially for indium. The boron concentration in II-tellurides is negligible, and its contribution to transport mechanisms has not been studied yet. For the last few years the authors have been developing a new technique to grow CdZnTe by the vertical Bridgman technique, taking advantage of encapsulation by means of boron oxide. In this way, crystals characterized by large single grains, low etch pit density, and high resistivity have been obtained. Recently, x-ray detectors with state-of-the-art performance have been produced from such crystals. Boron contamination, as a consequence of this growth method, is quite low but at least one order of magnitude above values obtained with other growth techniques. Besides being a low-cost technique which is also suitable for large-scale mass production, the encapsulated vertical Bridgman technique is quite useful to prevent dislocations, grain boundaries, and stacking faults; for these reasons, careful characterization was performed to understand the effect of boron both on the electrical properties and on the spectroscopic performance of the final crystals. Our characterization is mainly based on low-temperature photoluminescence in addition to electrical current-voltage measurements, photostimulated current, and x-ray spectroscopy. The results indicate that boron behaves like other group III elements; in fact, boron forms a complex that does not affect the good performance of our x-ray detectors, even if it shows some properties which are typical of A-centers.

Advanced methods for preparation and characterization of infrared detector materials

NASA Technical Reports Server (NTRS)

Broerman, J. G.; Morris, B. J.; Meschter, P. J.

1983-01-01

Crystals were prepared by the Bridgman-Stockbarger method with a wide range of crystal growth rates and temperature gradients adequate to prevent constitutional supercooling under diffusion-limited, steady-state, growth conditions. The longitudinal compositional gradients for different growth conditions and alloy compositions were calculated and compared with experimental data to develop a quantitative model of solute redistribution during the crystal growth of the alloys. Measurements were performed to ascertain the effect of growth conditions on radial compositional gradients. The pseudobinary HgTe-CdTe constitutional phase diagram was determined by precision differential-thermal-analysis measurements and used to calculate the segregation coefficient of Cd as a function of x and interface temperature. Experiments were conducted to determine the ternary phase equilibria in selected regions of the Hg-Cd-Te constitutional phase diagram. Electron and hole mobilities as functions of temperature were analyzed to establish charge-carrier scattering probabilities. Computer algorithms specific to Hg(1-x)CdxTe were developed for calculations of the charge-carrier concentration, charge-carrier mobilities, Hall coefficient, and Dermi Fermi energy as functions of x, temperature, ionized donor and acceptor concentrations, and neutral defect concentrations.

HRTEM Analysis of Crystallographic Defects in CdZnTe Single Crystal

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Determination of the Wetting Angle of Germanium and Germanium-Silicon Melts on Different Substrate Materials

NASA Technical Reports Server (NTRS)

Kaiser, Natalie; Croell, Arne; Szofran, F. R.; Cobb. S. D.; Dold, P.; Benz, K. W.

1999-01-01

During Bridgman growth of semiconductors detachment of the crystal and the melt meniscus has occasionally been observed, mainly under microgravity (microg) conditions. An important factor for detached growth is the wetting angle of the melt with the crucible material. High contact angles are more likely to result in detachment of the growing crystal from the ampoule wall. In order to achieve detached growth of germanium (Ge) and germanium-silicon (GeSi) crystals under 1g and microg conditions, sessile drop measurements were performed to determine the most suitable ampoule material as well as temperature dependence of the surface tension for GeSi. Sapphire, fused quartz, glassy carbon, graphite, SiC, pyrolytic Boron Nitride (pBN), AIN, and diamond were used as substrates. Furthermore, different cleaning procedures and surface treatments (etching, sandblasting, etc.) of the same substrate material and their effect on the wetting behavior were studied during these experiments. pBN and AIN substrates exhibited the highest contact angles with values around 170 deg.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Application of strong vertical magnetic fields to growth of II-VI pseudo-binary alloys - HgMnTe

NASA Astrophysics Data System (ADS)

Becla, Piotr; Han, Jian-Chiu; Motakef, Shahryar

1992-07-01

HgMnTe crystals are grown by the vertical Bridgman method in the presence of an applied vertical magnetic field of 30 kG. Reduction of convective intensity in the melt through application of the magnetic field is found to decrease radial macro-segregation and eliminate small-scale compositional undulations in the grown material; the axial compositional profile is found not to be influenced by the magnetic field. These observations are shown to be consistent with a previously proposed model for the residual convection present during growth of this and other similar materials.

Fluid flow analysis and vertical gradient freeze crystal growth in a travelling magnetic field

NASA Astrophysics Data System (ADS)

Lantzsch, R.; Grants, I.; Galindo, V.; Patzold, O.; Gerbeth, G.; Stelter, M.; Croll, A.

2006-12-01

In bulk crystal growth of semiconductors the concept of remote flow control by means of alternating magnetic fields has attracted considerable interest (see, e.g., te{1,2,3,4,5,6}). In this way the melt flow can be tailored for growth under optimised conditions to improve the crystal properties and/or the growth yield. A promising option is to apply an axially travelling magnetic wave to the melt (Travelling Magnetic Field - TMF). It introduces a mainly axial Lorentz force, which leads to meridional flow patterns. In recent numerical studies te{3}, te{6} the TMF has been recognised to be a versatile and efficient tool to control the heat and mass transport in the melt. For the Vertical Bridgman/Vertical Gradient Freeze (VB/VGF) growth, the beneficial effect of an adequately adjusted TMF-induced flow was clearly demonstrated in te{6} in terms of the reduction of thermal shear stress at the solid-liquid interface. In this paper, we present experimental and numerical results on the TMF driven convection in an isothermal model fluid as well as first VGF-TMF crystal growth experiments. The model investigations are focused on the transition from laminar to instationary flow conditions that should be avoided in crystal growth applications. The VGF experiments were aimed at growing Ga doped germanium single crystals under the influence of the travelling field in a newly developed VGF-TMF equipment. Figs 4, Refs 10.

Crystal growth of Bi{sub 2}Te{sub 3} and noble cleaved (0001) surface properties

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

Atuchin, V.V., E-mail: atuchin@thermo.isp.nsc.ru; Functional Electronics Laboratory, Tomsk State University, Tomsk 634050; Golyashov, V.A.

2016-04-15

A high quality Bi{sub 2}Te{sub 3} crystal has been grown by Bridgman method with the use of rotating heat field. The phase purity and bulk structural quality of the crystal have been verified by XRD analysis and rocking curve observation. The atomically smooth Bi{sub 2}Te{sub 3}(0001) surface with an excellent crystallographic quality is formed by cleavage in the air. The chemical and microstructural properties of the surface have been evaluated with RHEED, AFM, STM, SE and XPS. The Bi{sub 2}Te{sub 3}(0001) cleaved surface is formed by atomically smooth terraces with the height of the elemental step of ~1.04±0.1 nm, asmore » estimated by AFM. There is no surface oxidation process detected over a month keeping in the air at normal conditions, as shown by comparative core level photoelectron spectroscopy. - Graphical abstract: A high quality Bi{sub 2}Te{sub 3} crystal has been grown by Bridgman method with the use of rotating heat field and the Bi{sub 2}Te{sub 3}(0001) cleaved surface has been evaluated with RHEED, AFM, STM, SE and XPS. - Highlights: • High-quality Bi{sub 2}Te{sub 3} crystal of 10 mm in diameter and 50 mm long have been grown. • The high-purity cleaved Bi{sub 2}Te{sub 3}(0001) surface has been evaluated by RHEED, AFM, STM and XPS methods. • The Bi{sub 2}Te{sub 3} surface covered by atomically smooth (0001) terraces is chemically stable for a long time.« less

Benzil: 2-methyl-4-nitroaniline binary single crystals for nonlinear optical applications

NASA Astrophysics Data System (ADS)

Choi, Jaeho; Aggarwal, Mohan D.; Wang, Wen Shan; Penn, Benjamin G.; Frazier, Donald O.

1999-06-01

Benzil:MNA binary organic single crystals have been grown to overcome decomposition tendency and improve mechanical properties of 2-methyl-4-nitroaniline (MNA) which is known to be one of the best organic NLO material. Single crystals of binary system have grown using a transparent Bridgman- Stockbarger system which has fabricated to monitor the growth process. The growth conditions for the flat solid- liquid interface are optimized for the different dopant concentration of benzil. The melt in the self-sealing ampoule is maintained in liquid state without decomposition up to 2 weeks which allows us to grow 20 mm long single crystals. Hardness of 5wt% benzil:MNA is measured to be 13 Kg/mm2 which is 45% higher than benzil. The conversion efficiency of second-harmonic generation is found to be 1.5% with 4.5 mm interaction length. Since MNA is phase-matchable material, this efficiency could be comparable to commercial KDP. Surface quality of binary crystals has maintained its initial condition in air without absorption of water vapor which may be the main cause of surface degradation.

Growth of langasite via Bridgman technique along [ 0 0 0 1], [ 2 1¯ 1¯ 0] and [ 0 1 1¯ 1] for piezoelectric applications

NASA Astrophysics Data System (ADS)

Uda, Satoshi; Inaba, Hitoshi; Harada, Jiro; Hoshikawa, Keigo

2004-10-01

2-inch langasite (La 3Ga 5SiO 14) single crystals were grown for the first time via a vertical Bridgman method, assisted by the accelerated crucible rotation technique (ACRT) along [ 0 0 0 1] ( Z-axis), [ 2 1¯ 1¯ 0] ( X-axis) and [ 0 1 1¯ 1] (54°-rotated Y-axis) for piezoelectric applications. Because of the possible liquid immiscibility, incongruency and segregation, secondary phases other than langasite are formed during growth. The mode of occurrence of these phases was closely related to the interface instability that was specific to the growth direction. The formation of inclusions consisting of lanthanum gallate (LaGaO 3), aligned parallel to ( 0 1 1¯ 0), was associated with the constitutional supercooling. The residual products during the terminal transient were the mixture of gallium oxide (Ga 2O 3) and lanthanum gallate (LaGaO 3) or the mixture of gallium oxide and lanthanum silicate (La 2Si 2O 7) reflecting the position of the initial melt, relative to the tie line connecting the langasite solid solution with gallium oxide in the system of La 2O 3-Ga 2O 3-SiO 2. The homogeneity of the grown crystal was evaluated by the distribution of SAW velocities of the devices fabricated on the ( 0 1 1¯ 0) wafer, as well as by the uniformity of d-spacing of 0 5 5¯ 5.

Simplified numerical approach for estimation of effective segregation coefficient at the melt/crystal interface

NASA Astrophysics Data System (ADS)

Prostomolotov, A. I.; Verezub, N. A.; Voloshin, A. E.

2014-09-01

A thermo-gravitational convection and impurity transfer in the melt were investigated using a simplified numerical model for Bridgman GaSb(Te) crystal growth in microgravity conditions. Simplifications were as follows: flat melt/crystal interface, fixed melt sizes and only lateral ampoule heating. Calculations were carried out by Ansys®Fluent® code employing a two-dimensional Navier-Stokes-Boussinesq and heat and mass transfer equations in a coordinate system moving with the melt/crystal interface. The parametric dependence of the effective segregation coefficient Keff at the melt/crystal interface was studied for various ampoule sizes and for microgravity conditions. For the uprising one-vortex flow, the resulting dependences were presented as Keff vs. Vmax-the maximum velocity value. These dependences were compared with the formulas by Burton-Prim-Slichter's, Ostrogorsky-Muller's, as well as with the semi-analytical solutions.

Crystal growth of LiIn 1–xGa xSe 2 crystals

DOE PAGES

Wiggins, Brenden; Bell, Joseph; Woodward, Jonathan; ...

2016-10-22

Lithium containing chalcogenide single crystals have become very promising materials for photonics and radiation detection. Detection applications include nuclear nonproliferation, neutron science, and stellar investigations for the search of life. Synthesis and single crystal growth methods for lithium containing chalcogenide, specifically LiIn 1-xGa xSe 2, single crystals are discussed. This study elucidates the possibility of improving neutron detection by reducing the indium capture contribution; with the incorporation of the lithium-6 isotope, gallium substitution may overcome the neutron detection efficiency limitation of 6LiInSe 2 due to appreciable neutron capture by the indium-115 isotope. As a figure of merit, the ternary parentmore » compounds 6LiInSe 2 and 6LiGaSe 2 were included in this study. Quality crystals can be obtained utilizing the vertical Bridgman method to produce quaternary compounds with tunable optical properties. Here, quaternary crystals of varying quality depending on the gallium concentration, approximately 5 x 5 x 2 mm 3 or larger in volume, were harvested, analyzed and revealed tunable absorption characteristics between 2.8-3.4 eV.« less

Melt Stabilization of PbSnTe in a Magnetic Field

NASA Technical Reports Server (NTRS)

Fripp, Archibald L.; Debnam, William J.; Rosch, William; Chait, Arnon; Yao, Minwu; Szofran, Frank R.

1999-01-01

Both the experimental observation and numerical simulation indicate that the Bridgman growth of PbSnTe under the microgravity environment in space is still greatly influenced by buoyancy-induced convection. The application of a magnetic field during the semiconductor growth can dampen the convective flow in the metal-like melt. However, for Bridgman growth of PbSnTe on earth (with either vertical or horizontal configuration), both experimental observation and numerical modeling suggest that even with a strong magnetic furnace (5-Tesla constant axial magnetic field), the convective flow in the melt still cannot be sufficiently suppressed to reach the diffusion-controlled level. In order to completely dampen the buoyancy-induced convection on earth, estimates based on scaling analysis indicate that for common experimental conditions, an extremely high magnetic field is required, far beyond the capacity of the experimental apparatus currently available. Therefore, it is proposed that only the combination of microgravity environment and magnetic damping will produce the desired diffusion-controlled growth state for this particular material. The primary objectives of this study are to provide a quantitative understanding of the complex transport phenomena during solidification of non-dilute binarys, to furnish a numerical tool for furnace design and growth condition optimization, to provide estimates of the required magnetic field strength for low gravity growth, and to assess the role of magnetic damping for space and earth control of the double-diffusive convection. As an integral part of a NASA research program, our numerical simulation supports both the flight and ground-based experiments in an effort to bring together a complete picture of the complex physical phenomena involved in the crystal growth process. For Bridgman growth of PbSnTe under microgravity (with both vertical and horizontal configurations), the simulations suggest that a moderate axial magnetic field of only a few kilo-Gauss in strength could effectively eliminate buoyancy-induced convection in the melt and control solute segregation. Therefore, this work confirms the idea that the combination of microgravity environment and the magnetic damping will indeed be sufficient to produce the desired diffusion-controlled growth state for PbSnTe.

Thermoelectric properties of Ge 1-xSn xTe crystals grown by vertical Bridgman method

NASA Astrophysics Data System (ADS)

Wu, C. C.; Ferng, N. J.; Gau, H. J.

2007-06-01

Single crystals of Ge 1-xSn xTe compounds with x=0, 0.8, 0.9 and 1.0 were grown by vertical Bridgman method. The crystalline phase and stochiometry for these crystals were investigated by X-ray diffraction, metallographic microscope as well as electron-probe microanalysis (EPMA). Electrical property of the as-grown samples was characterized using room temperature resistivity and Hall measurements. The thermoelectric behaviors for the Ge 1-xSn xTe crystals were studied by means of thermal and carrier transport measurements. Temperature dependences of resistivity, Seebeck coefficient and thermal conductivity for the various compositions of Ge 1-xSn xTe were analyzed. A two-valence band model was proposed to describe the temperature dependence of thermoelectric property of the Ge 1-xSn xTe crystals. The dimensionless thermoelectric figure of merit ZT for the alloys was evaluated and discussed.

Crystal structure and thermal expansion of CsCaI3:Eu and CsSrBr3:Eu scintillators

NASA Astrophysics Data System (ADS)

Loyd, Matthew; Lindsey, Adam; Patel, Maulik; Koschan, Merry; Melcher, Charles L.; Zhuravleva, Mariya

2018-01-01

The distorted-perovskite scintillator materials CsCaI3:Eu and CsSrBr3:Eu prepared as single crystals have shown promising potential for use in radiation detection applications requiring a high light yield and excellent energy resolution. We present a study using high temperature powder X-ray diffraction experiments to examine a deleterious high temperature phase transition. High temperature phases were identified through sequential diffraction pattern Rietveld refinement in GSAS II. We report the linear coefficients of thermal expansion for both high and low temperature phases of each compound. Thermal expansion for both compositions is greatest in the [0 0 1] direction. As a result, Bridgman growth utilizing a seed oriented with the [0 0 1] along the growth direction should be used to mitigate thermal stress.

Gettering of donor impurities by V in GaAs and the growth of semi-insulating crystals

NASA Technical Reports Server (NTRS)

Ko, K. Y.; Lagowski, J.; Gatos, H. C.

1989-01-01

Vanadium added to the GaAs melt getters shallow donor impurities (Si and S) and decreases their concentration in the grown crystals. This gettering is driven by chemical reactions in the melt rather than in the solid. Employing V gettering, reproducibly semi-insulating GaAs were grown by horizontal Bridgman and liquid-encapsulated Czochralski techniques, although V did not introduce any midgap energy levels. The compensation mechanism in these crystals was controlled by the balance between the native midgap donor EL2 and residual shallow acceptors. Vanadium gettering contributed to the reduction of the concentration of shallow donors below the concentration of acceptors. The present findings clarify the long-standing controversy on the role of V in achieving semi-insulating GaAs.

Crystal Growth of II-VI Semiconducting Alloys by Directional Solidification

NASA Technical Reports Server (NTRS)

Lehoczky, Sandor L.; Szofran, Frank R.; Su, Ching-Hua; Cobb, Sharon D.; Scripa, Rosalia A.; Sha, Yi-Gao

1999-01-01

This research study is investigating the effects of a microgravity environment during the crystal growth of selected II-VI semiconducting alloys on their compositional, metallurgical, electrical and optical properties. The on-going work includes both Bridgman-Stockbarger and solvent growth methods, as well as growth in a magnetic field. The materials investigated are II-VI, Hg(1-x)Zn(x)Te, and Hg(1-x)Zn(x)Se, where x is between 0 and 1 inclusive, with particular emphasis on x-values appropriate for infrared detection and imaging in the 5 to 30 micron wavelength region. Wide separation between the liquidus and solidus of the phase diagrams with consequent segregation during solidification and problems associated with the high volatility of one of the components (Hg), make the preparation of homogeneous, high-quality, bulk crystals of the alloys an extremely difficult nearly an impossible task in a gravitational environment. The three-fold objectives of the on-going investigation are as follows: (1) To determine the relative contributions of gravitationally-driven fluid flows to the compositional redistribution observed during the unidirectional crystal growth of selected semiconducting solid solution alloys having large separation between the liquidus and solidus of the constitutional phase diagram; (2) To ascertain the potential role of irregular fluid flows and hydrostatic pressure effects in generation of extended crystal defects and second-phase inclusions in the crystals; and, (3) To obtain a limited amount of "high quality" materials needed for bulk crystal property characterizations and for the fabrication of various device structures needed to establish ultimate material performance limits. The flight portion of the study was to be accomplished by performing growth experiments using the Crystal Growth Furnace (CGF) manifested to fly on various Spacelab missions.

Single crystal growth and surface chemical stability of KPb2Br5

NASA Astrophysics Data System (ADS)

Atuchin, V. V.; Isaenko, L. I.; Kesler, V. G.; Tarasova, A. Yu.

2011-03-01

Single crystal of KPb2Br5 has been grown using the Bridgman technique. Initially the synthesis of stoichiometric KPb2Br5 compound was performed from high purity bromide salts. Electronic structure of KPb2Br5 has been determined with X-ray photoelectron spectroscopy for powdered sample fabricated by grinding in air. Drastic chemical interaction of KPb2Br5 with atmosphere has not been detected. Chemical bonding in potassium- and lead-containing bromides is considered using binding energy differences ΔK=(BE K 2p3/2-BE Br 3d) and ΔPb=(BE Pb 4f7/2-BE Br 3d), respectively, as representative parameters.

Bridgman growth of semiconductors

NASA Technical Reports Server (NTRS)

Carlson, F. M.

1985-01-01

The purpose of this study was to improve the understanding of the transport phenomena which occurs in the directional solidification of alloy semiconductors. In particular, emphasis was placed on the strong role of convection in the melt. Analytical solutions were not deemed possible for such an involved problem. Accordingly, a numerical model of the process was developed which simulated the transport. This translates into solving the partial differential equations of energy, mass, species, and momentum transfer subject to various boundary and initial conditions. A finite element method with simple elements was initially chosen. This simulation tool will enable the crystal grower to systematically identify and modify the important design factors within her control to produce better crystals.

Numerical and analytical modelling of the MHD buoyancy-driven flow in a Bridgman crystal growth configuration

NASA Astrophysics Data System (ADS)

Davoust, L.; Moreau, R.; Cowley, M. D.; Tanguy, P. A.; Bertrand, F.

1997-10-01

We present analytical and numerical models of magnetohydrodynamic(MHD) buoyancy-driven flow within the liquid pool of a horizontal Bridgman crystal growth furnace, under the influence of a uniform vertical magnetic field B0. A horizontal differentially heated cylinder, whose aspect ratio (radius to length) is small enough for a fully developed regime to be established in the central core, is considered. With Hartmann layers remaining electrically inactive, a modified Rayleigh number RaG, which is the ration of the ordinary Rayleigh number to the square of the Hartmann number, is found to control the MHD reorganisation of the flow. This modified Rayleigh number is a measure of the importance of thermal convection relative to diffusion if velocity is estimated from the balance between the torques of buoyancy and the Laplace force. When RaG is much smaller than unity (quasi-diffusive regime), an analytical modelling of the flow, based on a power series of RaG, demonstrates that this balance requires secondary vortices within vertical mid-planes of the cylinder, both within the core flow and near the end walls. A 3-D numerical calculation of the flow provides evidence of the transition from a convective MHD flow (when RaG is still of the order of unity) to the quasi-diffusive flow, analytically studied. Indeed, this transition takes the form of a rather complex 3-D MHD organisation of the flow which is due to the nonuniformity of the axial temperature gradient along the cylinder.

Crystal growth and characterization of europium doped KCaI3, a high light yield scintillator

NASA Astrophysics Data System (ADS)

Lindsey, Adam C.; Zhuravleva, Mariya; Stand, Luis; Wu, Yuntao; Melcher, Charles L.

2015-10-01

The presented study reports on the spectroscopic characteristics of a new high performance scintillation material KCaI3:Eu. The growth of ∅ 17 mm boules using the Bridgman-Stockbarger method in fused silica ampoules is demonstrated to produce yellow tinted, yet transparent single crystals suitable for use in spectroscopic applications due to very promising performance. Scintillation light yield of 72,000 ± 3000 ph/MeV and energy resolution of 3% (FWHM) at 662 keV and 6.1% at 122 keV was obtained from small single crystals of approximately 15 mm3. For a much larger 3.8 cm3 detector, 4.4% and 7.3% for the same energy. Proportionality of the scintillation response to the energy of ionizing radiation is within 96% of the ideal response over an energy range of 14-662 keV. The high light yield and energy resolution of KCaI3:Eu make it suitable for potential use in domestic security applications requiring radionuclide identification.

Crystal growth and characterization of Hg-based chalcogenide compounds (Conference Presentation)

NASA Astrophysics Data System (ADS)

He, Yihui; Lin, Wenwen; Syrigos, Jonathan C.; Wang, Peng Li; Islam, Saiful M.; McCall, Kyle M.; Kostina, Svetlana S.; Liu, Zhifu; Wessels, Bruce W.; Kanatzidis, Mercouri G.

2016-09-01

In this work, two Hg-based chalcogenides were investigated in detail to reveal their potential capability of radiation detection at room temperature (RT). Cs2Hg6S7, with a bandgap of 1.63 eV, which is designed by the dimensional reduction theory proposed by our group, were prepared and characterized. α-HgS, with a bandgap of 2.10 eV, as a precursor used for the ternary compound synthesis, was also proposed and further investigated. For Cs2Hg6S7, the crystals tended to crystallize into needle form with small grains. Here, the conditions of Bridgman melt growth were optimized to obtain relatively large single crystals. The slight excess of Cs2S as a fluxing agent during growth was found to facilitate better crystallization and large grains. Interestingly, no inclusion or secondary phase was found in the as-grown single crystals. The improvement of bulk resistivity from 10^6 Ωcm to 10^8 Ωcm was also achieved through the control of stoichiometry during crystal growth. For α-HgS crystals, both physical vapor transport and chemical vapor transport methods have been applied. By modifying the transport temperature and transport agent, single crystal with size about 3x1.5 mm^2 was grown with resistivity higher than 10^11 Ωcm. Photoluminescence (PL) revealed that multiple peaks observed in the 1.6-2.3 eV range and excitonic peak from for α-HgS single crystals were observed indicating good crystalline quality. Finally, the planar detectors for both crystals were tested under Co57 gamma ray source. Both of the crystals showed reasonable gamma ray response, while α-HgS crystals could respond at a relatively higher counting rate.

Convective Influence on Radial Segregation During Unidirectional Solidification of the Binary Alloy HgCdTe

NASA Technical Reports Server (NTRS)

Watring, D. A.; Gillies, D. C.; Lehoczky, S. L.; Szofran, F. R.; Alexander, H.

1996-01-01

In order to simulate the space environment for basic research into the crystal growth mechanism, Hg(0.8)Cd(0.2)Te crystals were grown by the vertical Bridgman-Stockbarger method in the presence of an applied axial magnetic field. The influence of convection, by magneto hydrodynamic damping, on mass transfer in the melt and segregation at the solid-liquid interface was investigated by measuring the axial and radial compositional variations in the grown samples. The reduction of convective mixing in the melt through the application of the magnetic field is found to have a large effect on radial segregation and interface morphology in the grown crystals. Direct comparisons are made with a Hg(0.8)Cd(0.2)Te crystal grown without field and also in the microgravity environment of space during the second United States Microgravity Payload Mission (USMP-2).

An unusual crystal growth method of the chalcohalide semiconductor, β-Hg 3S 2Cl 2: A new candidate for hard radiation detection

DOE PAGES

Wibowo, Arief C.; Malliakas, Christos D.; Li, Hao; ...

2016-03-16

Here, we assess the mercury chalcohalide compound, β-Hg 3S 2Cl 2, as a potential semiconductor material for X-ray and γ-ray detection. It has a high density (6.80 g/cm 3) and wide band gap (2.56 eV) and crystallizes in the cubic Pm4more » $$\\bar{3}$$n space group with a three-dimensional structure comprised of [Hg 12S 8] cubes with Cl atoms located within and between the cubes, featuring a trigonal pyramidal SHg3 as the main building block. First-principle electronic structure calculations at the density functional theory level predict that the compound has closely lying indirect and direct band gaps. We have successfully grown transparent, single crystals of β-Hg 3S 2Cl 2 up to 7 mm diameter and 1 cm long using a new approach by the partial decomposition of the quaternary Hg 3Bi 2S 2Cl 8 compound followed by the formation of β-Hg 3S 2Cl 2 and an impermeable top layer, all happening in situ during vertical Bridgman growth. The decomposition process was optimized by varying peak temperatures and temperature gradients using a 2 mm/h translation rate of the Bridgman technique. Formation of the quaternary Hg 3Bi 2S 2Cl 8 followed by its partial decomposition into β-Hg 3S 2Cl 2 was confirmed by in situ temperature-dependent synchrotron powder diffraction studies. The single crystal samples obtained had resistivity of 10 10 Ω·cm and mobility-lifetime products of electron and hole carriers of 1.4(4) × 10 –4 cm 2/V and 7.5(3) × 10 –5 cm 2/V, respectively. Further, an appreciable Ag X-ray photoconductivity response was observed showing the potential of β-Hg 3S 2Cl 2 as a hard radiation detector material.« less

Analysis of the low gravity tolerance of Bridgman-Stockbarger crystal growth. I - Steady and impulse accelerations

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.; Ouazzani, Jalil; Rosenberger, Franz

1989-01-01

The effects of steady and impulse-type residual accelerations on dopant distributions during directional solidification in 2D and 3D 'generic' models of the Bridgman-Stockbarger technique are investigated using numerical methods. The calculations are based on the thermophysical properties of molten germanium doped with a low concentration of gallium. A Chebyshev collocation pseudospectral method is used for the solution of the governing momentum-, mass-, species-, and heat-transfer equations. Only convection caused by temperature gradients is considered. It is found that lateral nonuniformity in composition is very sensitive to the orientation of the steady component of the residual gravity vector and to the particular operating conditions under consideration. It is also found that laterally or radially averaged composition profiles are alone insufficient to describe the extent of residual convection in a spacecraft environment. The effects of impulse-type disturbances can be severe and can extend for times on the order of 1000 sec after the termination of the impulse.

Modelling of directional solidification of BSO

NASA Astrophysics Data System (ADS)

Lin, Chenting; Motakef, Shahryar

1993-03-01

A thermo-fluid model for vertical Bridgman growth of bismuth silicon oxide (BSO) as model material for semi-transparent, low thermal conductivity oxides is developed. Internal radiative heat transfer, together with convective and conductive heat transfer are considered in this model. Due to the strong internal thermal radiation within the grown crystal, the growth interface is highly convex into the melt, instead of being concave as is the case for opaque materials with the thermal conductivity of the melt larger than that of the solid. Reduction of the growth interface non-planarity through variations in the growth configuration is investigated. A furnace temperature profile consisting of a steep gradient on the melt side and shallow gradient on the solid side of the charge is found to be the most effective approach.

A Chebyshev Collocation Method for Moving Boundaries, Heat Transfer, and Convection During Directional Solidification

NASA Technical Reports Server (NTRS)

Zhang, Yiqiang; Alexander, J. I. D.; Ouazzani, J.

1994-01-01

Free and moving boundary problems require the simultaneous solution of unknown field variables and the boundaries of the domains on which these variables are defined. There are many technologically important processes that lead to moving boundary problems associated with fluid surfaces and solid-fluid boundaries. These include crystal growth, metal alloy and glass solidification, melting and name propagation. The directional solidification of semi-conductor crystals by the Bridgman-Stockbarger method is a typical example of such a complex process. A numerical model of this growth method must solve the appropriate heat, mass and momentum transfer equations and determine the location of the melt-solid interface. In this work, a Chebyshev pseudospectra collocation method is adapted to the problem of directional solidification. Implementation involves a solution algorithm that combines domain decomposition, finite-difference preconditioned conjugate minimum residual method and a Picard type iterative scheme.

Opportunity for academic research in a low-gravity environment - Crystal growth

NASA Technical Reports Server (NTRS)

Matthiesen, D. H.; Wargo, M. J.; Witt, A. F.

1986-01-01

The history of basic and applied research on crystal growth (CG), especially of semiconductor materials, is reviewed, stressing the dominance (at least in the U.S.) of industrial R&D projects over academic programs and the need for more extensive fundamental investigations. The NASA microgravity research program and the recommendations of the University Space Research Association are examined as they affect the availability of space facilities for academic CG research. Also included is a report on ground experiments on the effectiveness of magnetic fields in controlling vertical Bridgman CG and melt stability, using the apparatus employed in the Apollo-Soyuz experiments (Witt et al., 1978); the results are presented in graphs and briefly characterized. The role of NASA's microgravity CG program in stimulating academic work on CG, the importance of convection effects, CG work on materials other than semiconductors, and NSF support of CG research are discussed in a comment by R. F. Sekerka.

Crystal growth and scintillation properties of potassium strontium bromide

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Wei, H.; Melcher, C. L.

2015-08-01

In this work, potassium strontium bromide activated with divalent europium, (KSr2Br5:Eu) has been studied. It has a monoclinic crystal structure and a density of 3.98 g/cm3. Two single crystals of KSr2Br5 doped with 5% Eu2+, with diameters of 13 mm and 22 mm, were grown in a two zone transparent furnace via the Bridgman technique. The X-ray excited emission spectrum consisted of a single peak at ∼427 nm due to the 5d-4f transition in Eu2+. The measured light yield and energy resolution at 662 keV was 75,000 ph/MeV and 3.5%. At low energies KSr2Br5:Eu 5% also displays good energy resolution, 6.7% at 122 keV and 7.9% at 59.5 keV.

Forced convection in vertical Bridgman configuration with the submerged heater

NASA Astrophysics Data System (ADS)

Meyer, S.; Ostrogorsky, A. G.

1997-02-01

Ga-doped Ge single crystals were grown in vertical Bridgman configuration, using the submerged heater method (SHM). When used without rotation, the submerged heater drastically reduces convection at the solid-liquid interface. When the submerged heater is set in to rotation or oscillatory rotation, it acts as a centrifugal viscous pump, inducing forced convection (radial-inward flow) along the interface. The flow produced by a rotation and oscillatory rotation of the submerged heater was visualized using a 1 : 1 scale model. The vigorous mixing produced by the oscillatory rotation creates a nearly perfectly stirred melt, and yields a uniform lateral distribution of the dopant. The crystals were free of unintentionally produced striae.

Crystal growth and fluid mechanics problems in directional solidification

NASA Technical Reports Server (NTRS)

Tanveer, Saleh; Baker, Gregory R.; Foster, Michael R.

1994-01-01

Broadly speaking, our efforts have been concentrated in two aspects of directional solidification: (A) a more complete theoretical understanding of convection effects in a Bridgman apparatus; and (B) a clear understanding of scalings of various features of dendritic crystal growth in the sensitive limit of small capillary effects. For studies that fall within class A, the principal objectives are as follows: (A1) Derive analytical formulas for segregation, interfacial shape and fluid velocities in mathematically amenable asymptotic limits. (A2) Numerically verify and extend asymptotic results to other ranges of parameter space with a view to a broader physical understanding of the general trends. With respect to studies that fall within class B, the principal objectives include answering the following questions about dendritic crystal growth: (B1) Are there unsteady dendrite solutions in 2-D to the completely nonlinear time evolving equations in the small surface tension limit with only a locally steady tip region with well defined tip radius and velocity? Is anisotropy in surface tension necessary for the existence of such solutions as it is for a true steady state needle crystal? How does the size of such a local region depend on capillary effects, anisotropy and undercooling? (B2) How do the different control parameters affect the nonlinear amplification of tip noise and dendritic side branch coarsening?

Crystal growth, structural, low temperature thermoluminescence and mechanical properties of cubic fluoroperovskite single crystal (LiBaF3)

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Ramasamy, P.; Ramaseshan, R.; Kim, H. J.; Kim, Sunghwan; Bhagavannarayana, G.; Cheon, Jong-Kyu

2017-10-01

Polycrystalline compounds of LiBaF3 were synthesized using conventional solid state reaction route and the phase purity was confirmed using powder X-ray diffraction technique. Using vertical Bridgman technique single crystal was grown from melt. Rocking curve measurements have been carried out to study the structural perfection of the grown crystal. The single peak of diffraction curve clearly reveals that the grown crystal was free from the structural grain boundaries. The low temperature thermoluminescence of the X-ray irradiated sample has been analyzed and found four distinguishable peaks having maximum temperatures at 18, 115, 133 and 216 K. Activation energy (E) and frequency factor (s) for the individual peaks have been studied using Peak shape method and the computerized curve fitting method combining with the Tmax- TStop procedure. Nanoindentation technique was employed to study the mechanical behaviour of the crystal. The indentation modulus and Vickers hardness of the grown crystal have values of 135.15 GPa and 680.81 respectively, under the maximum indentation load of 10 mN.

Experimental observation of the influence of furnace temperature profile on convection and segregation in the vertical Bridgman crystal growth technique

NASA Technical Reports Server (NTRS)

Neugebauer, G. T.; Wilcox, William R.

1992-01-01

Azulene-doped naphthalene was directionally solidified during the vertical Bridgman-Stockbarger technique. Doping homogeneity and convection were determined as a function of the temperature profile in the furnace and the freezing rate. Convection velocities were two orders of magnitude lower when the temperature increased with height. Rarely was the convection pattern axisymmetric, even though the temperature varied less than 0.1 K around the circumference of the growth ampoule. Correspondingly the cross sectional variation in azulene concentration tended to be asymmetric, especially when the temperature increased with height. This cross sectional variation changed dramatically along the ingot, reflecting changes in convection presumably due to the decreasing height of the melt. Although there was large scatter and irreproducibility in the cross sectional variation in doping, this variation tended to be least when the growth rate was low and the convection was vigorous. It is expected that compositional variations would also be small at high growth rates with weak convection and flat interfaces, although this was not investigated in the present experiments. Neither rotation of the ampoule nor deliberate introduction of thermal asymmetries during solidification had a significant influence on cross sectional variations in doping. It is predicted that slow directional solidification under microgravity conditions could produce greater inhomogeneities than on Earth. Combined use of microgravity and magnetic fields would be required to achieve homogeneity when it is necessary to freeze slowly in order to avoid constitutional supercooling.

Optimization of the photorefractivity in II-IV semiconductors. Final report, March 1996--March 1997

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

Jagannathan, G.V.; Trivedi, S.B.; Kutcher, S.W.

1998-11-01

This work was aimed at optimization of the photorefractivity in the II-VI semiconductors CdTe, ZnTe and Cd{sub x{minus}1}Zn{sub (x)}Te for real-time optical signal processing applications at near infrared wavelengths. During this work, several crystals of ZnTe, CdTe and Cd{sub x{minus}1}Zn{sub (x)}Te were grown. Crystal growth of ZnTe and CdTe was carried out using low supersaturation nucleation and `contactless` growth by Vertical Physical Vapor Transport (PVT) in closed ampoules and the CdTe and Cd{sub x{minus}1}Zn{sub (x)}Te crystals were grown using the vertical Bridgman technique. The quality of the crystals grown during this work was evaluated based on optical, electrical and structuralmore » characterization. Infrared microscopy was used to examine the internal crystalline structure of the samples. Most of the crystals grown during this work exhibited photorefractivity and photoconductivity. The resistivity of the vanadium doped crystals under dark conditions was found to be between 10 {sup 8} to 10 {sup 10} ohms cm. The resistivity decreased significantly in the presence of illumination indicating that the crystals were highly photoconductive. The photorefractive properties of the crystals grown during this project were characterized by two beam coupling. All of the measurements revealed a strong photorefractive nonlinear effect.« less

Crystal growth and characterization of undoped and Dy-doped TlPb2Br5 for infrared lasers and nuclear radiation detection

NASA Astrophysics Data System (ADS)

Hömmerich, U.; Brown, E.; Kabir, A.; Hart, D.; Trivedi, S. B.; Jin, F.; Chen, H.

2017-12-01

We report results of the crystal growth and characterization of undoped and Dy-doped TlPb2Br5 for applications in infrared (IR) lasers and nuclear radiation detection. TlPb2Br5 (TPB) was synthesized from commercial starting materials of PbBr2 and TlBr and further purified through a combination of zone-refinement and directional solidification. For doping experiments, 2 wt% of DyBr3 was added to the purified TPB material. Crystal growth of TPB and Dy: TPB was carried out in a two-zone tube furnace by a vertical Bridgman method. Following optical excitation at ∼1.36 μm, the Dy: TPB crystal exhibited efficient mid-IR emission bands centered at 2.87 μm and 4.35 μm with room-temperature lifetimes of 9.5 ms and 5.2 ms, respectively. The peak emission cross-sections were determined to be ∼0.8 × 10-20 cm2 and ∼0.5 × 10-20 cm2, respectively, which makes Dy: TPB a promising candidate for mid-IR laser applications. Besides its potential as a solid-state laser host, an undoped TPB crystal was also tested for gamma-ray detection. Using Cs-137 and Am-241 sources resulted in energy resolutions for gamma-rays as good as 1-2% (FWHM) at room-temperature under non-optimized conditions.

Characterization of high-resistivity CdTe and Cd0.9Zn0.1Te crystals grown by Bridgman method for radiation detector applications

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Krishna, Ramesh M.; Pak, Rahmi O.; Mannan, Mohammad A.

2014-09-01

CdTe and Cd0.9Zn0.1Te (CZT) crystals have been studied extensively for various applications including x- and γ-ray imaging and high energy radiation detectors. The crystals were grown from zone refined ultra-pure precursor materials using a vertical Bridgman furnace. The growth process has been monitored, controlled, and optimized by a computer simulation and modeling program developed in our laboratory. The grown crystals were thoroughly characterized after cutting wafers from the ingots and processed by chemo-mechanical polishing (CMP). The infrared (IR) transmission images of the post-treated CdTe and CZT crystals showed average Te inclusion size of ~10 μm for CdTe and ~8 μm for CZT crystal. The etch pit density was ≤ 5×104 cm-2 for CdTe and ≤ 3×104 cm-2 for CZT. Various planar and Frisch collar detectors were fabricated and evaluated. From the current-voltage measurements, the electrical resistivity was estimated to be ~ 1.5×1010 Ω-cm for CdTe and 2-5×1011 Ω-cm for CZT. The Hecht analysis of electron and hole mobility-lifetime products (μτe and μτh) showed μτe = 2×10-3 cm2/V (μτh = 8×10-5 cm2/V) and 3-6×10-3 cm2/V (μτh = 4- 6×10-5 cm2/V) for CdTe and CZT, respectively. Detectors in single pixel, Frisch collar, and coplanar grid geometries were fabricated. Detectors in Frisch grid and guard-ring configuration were found to exhibit energy resolution of 1.4% and 2.6 %, respectively, for 662 keV gamma rays. Assessments of the detector performance have been carried out also using 241Am (60 keV) showing energy resolution of 4.2% FWHM.

Crystal Growth and Scintillation Properties of $${\\rm Cs}_{2}{\\rm NaGdBr}_{6}{:}{\\rm Ce}^{3+}$$

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

Yang, Pin; Zhou, Xiaowang; Deng, Haoran

2013-04-02

Single crystals of Cs 2NaGdBr 6 with different Ce +3 activator concentrations were grown by a two-zone Bridgman method. This new compound belongs to a large elpasolite halide (A 2BLnX 6) family. Many of these elpasolite compounds have shown high luminosity, good energy resolution and excellent proportionality in comparison to traditional scintillators such as CsI and NaI; therefore, they are particularly attractive for gamma-ray spectroscopy applications. This study investigated the scintillator properties of Cs 2NaGdBr 6:Ce +3 crystals as a new material for radiation detection. Special focus has been placed on the effects of activator concentration (0 to 50 mol.%)more » on the photoluminescence responses. Results of structural refinement, photoluminescence, radioluminescence, lifetime and proportionality measurements for this new compound are reported.« less

Stability of Detached Solidification

NASA Technical Reports Server (NTRS)

Mazuruk, K.; Volz, M. P.; Croell, A.

2009-01-01

Bridgman crystal growth can be conducted in the so-called "detached" solidification regime, where the growing crystal is detached from the crucible wall. A small gap between the growing crystal and the crucible wall, of the order of 100 micrometers or less, can be maintained during the process. A meniscus is formed at the bottom of the melt between the crystal and crucible wall. Under proper conditions, growth can proceed without collapsing the meniscus. The meniscus shape plays a key role in stabilizing the process. Thermal and other process parameters can also affect the geometrical steady-state stability conditions of solidification. The dynamic stability theory of the shaped crystal growth process has been developed by Tatarchenko. It consists of finding a simplified autonomous set of differential equations for the radius, height, and possibly other process parameters. The problem then reduces to analyzing a system of first order linear differential equations for stability. Here we apply a modified version of this theory for a particular case of detached solidification. Approximate analytical formulas as well as accurate numerical values for the capillary stability coefficients are presented. They display an unexpected singularity as a function of pressure differential. A novel approach to study the thermal field effects on the crystal shape stability has been proposed. In essence, it rectifies the unphysical assumption of the model that utilizes a perturbation of the crystal radius along the axis as being instantaneous. It consists of introducing time delay effects into the mathematical description and leads, in general, to stability over a broader parameter range. We believe that this novel treatment can be advantageously implemented in stability analyses of other crystal growth techniques such as Czochralski and float zone methods.

Transient segregation behavior in Cd1-xZnxTe with low Zn content-A qualitative and quantitative analysis

NASA Astrophysics Data System (ADS)

Neubert, M.; Jurisch, M.

2015-06-01

The paper analyzes experimental compositional profiles in Vertical Bridgman (VB, VGF) grown (Cd,Zn)Te crystals, found in the literature. The origin of the observed axial ZnTe-distribution profiles is attributed to dendritic growth after initial nucleation from supercooled melts. The analysis was done by utilizing a boundary layer model providing a very good approximation of the experimental data. Besides the discussion of the qualitative results also a quantitative analysis of the fitted model parameters is presented as far as it is possible by the utilized model.

Luminescence properties of ZnxMg1-xSe layers

NASA Astrophysics Data System (ADS)

Bala, Waclaw; Firszt, Franciszek; Dzik, Janusz; Gapinski, Adam; Glowacki, Grzegorz

1995-10-01

This work deals with the study of luminescence properties of ZnxMg1-xSe layers prepared by different methods. ZnxMg1-xSe mixed crystal layers were obtained by: (a) thermal diffusion of Mg metal in the temperature range 1050 K - 1200 K into ZnSe single crystal grown by Bridgman method, and (b) epitaxial growth on (001) GaAs and (111) ZnTe substrates by MBE using elemental Zn, Se and Mg sources. The luminescence spectra of ZnxMg1-xSe layers grown on (001) GaAs and (111) ZnTe substrates are dominated by narrow blue and violet emission bands with maxima positioned at about 3.05 - 3.28 eV, 2.88 - 3.04 eV, and 2.81 - 2.705 eV.

Advances in the growth of alkaline-earth halide single crystals for scintillator detectors

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

Boatner, Lynn A; Ramey, Joanne Oxendine; Kolopus, James A

2014-01-01

Alkaline-earth scintillators such as strontium iodide and other alkaline-earth halides activated with divalent europium represent some of the most efficient and highest energy resolution scintillators for use as gamma-ray detectors in a wide range of applications. These applications include the areas of nuclear nonproliferation, homeland security, the detection of undeclared nuclear material, nuclear physics and materials science, medical diagnostics, space physics, high energy physics, and radiation monitoring systems for first responders, police, and fire/rescue personnel. Recent advances in the growth of large single crystals of these scintillator materials hold the promise of higher crystal yields and significantly lower detector productionmore » costs. In the present work, we describe new processing protocols that, when combined with our molten salt filtration methods, have led to advances in achieving a significant reduction of cracking effects during the growth of single crystals of SrI2:Eu2+. In particular, we have found that extended pumping on the molten crystal-growth charge under vacuum for time periods extending up to 48 hours is generally beneficial in compensating for variations in the alkaline-earth halide purity and stoichiometry of the materials as initially supplied by commercial sources. These melt-pumping and processing techniques are now being applied to the purification of CaI2:Eu2+ and some mixed-anion europium-doped alkaline-earth halides prior to single-crystal growth by means of the vertical Bridgman technique. The results of initial studies of the effects of aliovalent doping of SrI2:Eu2+ on the scintillation characteristics of this material are also described.« less

Analysis of Radial Segregation in Directionally Solidified Hg(0.89)Mn(0.11)Te

NASA Technical Reports Server (NTRS)

Price, M. W.; Scripa, R. N.; Szofran, F. R.; Motakef, S.; Hanson, B.

2003-01-01

Bridgman growth experiments were performed on Hg(0.89)Mn(0.11)Te (MMT) to determine the extent of radial Manganese segregation during directional solidification. MMT crystals were directionally solidified at rates of 0.09 and 0.18 p d s and in axial thermal gradients of 83 and 68"C/cm. Wavelength Dispersive Spectroscopy (WDS) and Fourier Transform Infra-Red (FTIR) analytical techniques were used to determine the radial homogeneity in all boules and the deflection of the solid-liquid interface (SLI) in two boules that were rapidly quenched after 5 to 6 cm of directional solidification. For all growth runs, the measured radial coinpositional variations were on the order of 0.01 molar percent MnTe in the steady state region of growth. Comparison of the measured radial compositional results of the crystals to predicted values in the diffusion-limited regime indicate a strong influence of convection near the solid-liquid interface. This conclusion is supported by the weak influence of the translation rates and axial thermal gradients utilized in this study upon radial compositional homogeneity.

Control of Meridional Flow in Circular Cylinders by a Travelling Axial Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, K.; Ramachandran, N.; Volz, M. P.

1999-01-01

Convective flow in a Bridgman or float zone configuration significantly affects the interface shape and segregation phenomena. While the primary causative factor for this flow is buoyancy induced convection in an enclosed Bridgman melt, the presence of a free surface gives rise to surface tension driven flows in the floating zone processing of melts. It is of interest to curtail these flows in order to realize near quiescent growth conditions that have shown to result in crystals with good longitudinal and radial homogeneity and thereby of better overall quality. While buoyancy effects can be reduced by careful processing in a low gravity (space) environment, the reduction of Marangoni flows due to surface tension variations is not that straight forward. Attempts have been made with some limited success with the use of external fields to affect the melt thermo-fluid behavior. The use of a static magnetic field that reduces convective contamination through the effects of a non-intrusively induced, dissipative Lorentz force in an electrically conducting melt is one such approach. Experiments have shown that axial fields of the order of 5 Tesla can significantly eliminate convection and yield close to diffusion limited crystal growth conditions. The generation and use of such high magnetic fields require substantial hardware and incur significant costs for its operation. Lately, the use of rotating magnetic fields has been tested in semiconductor crystal growth. The method is fairly well known and commonly used in metal processing but its adaptation to crystal growth of semiconductors is fairly recent. The elegance of the technique rests in its low power requirement (typically 10-20 milli-Tesla at 50-400 Hz) and its efficacy in curtailing deleterious temperature fluctuations in the melt. A rotating magnetic field imposes a rotational force and thereby induces a circulation within the melt that tends to dominate other sporadic convective effects. Thus a known low level of convective flow is introduced into the system. A new novel variation of the Lorentz force mechanism is proposed and investigated in this study. Since one of the desired process conditions in melt crystal growth is the minimization of convective effects, this investigation examines the use of an external field of magnetic origin to counteract existing convective flow within the melt. This is accomplished by utilizing a running or traveling axial magnetic wave in the system. The concept is similar to the use of vibrational means in order to induce streaming flows that oppose buoyant or surface tension driven convection in the system. The rotation direction as well as the magnitude (strength) of this circulation can be easily controlled by external inputs thus affording a direct means of controlling the developing shape of the crystallizing front (interface). The theoretical model of this technique is fully developed and presented in this paper. Results from the solution of the developed governing equations and boundary conditions are also presented. An experimental demonstration of the concept is presented through the suppression of natural convective flow in a mercury column. Implications to crystal growth systems will be fully explored in the final manuscript.

Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions

NASA Technical Reports Server (NTRS)

Gandin, Charles-Andre; Ratke, Lorenz

2008-01-01

The Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MSL-CETSOL and MICAST) are two investigations which supports research into metallurgical solidification, semiconductor crystal growth (Bridgman and zone melting), and measurement of thermo-physical properties of materials. This is a cooperative investigation with the European Space Agency (ESA) and National Aeronautics and Space Administration (NASA) for accommodation and operation aboard the International Space Station (ISS). Research Summary: Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing (CETSOL) and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST) are two complementary investigations which will examine different growth patterns and evolution of microstructures during crystallization of metallic alloys in microgravity. The aim of these experiments is to deepen the quantitative understanding of the physical principles that govern solidification processes in cast alloys by directional solidification.

Growth experiment of narrow band-gap semiconductor PbSnTe single crystals in space (M-1)

NASA Technical Reports Server (NTRS)

Yamada, Tomoaki

1993-01-01

An experiment on crystal growth of Pb(1-x)Sn(x)Te in microgravity is planned. This material is an alloy of the compound semiconductors PbTe and SnTe. It is a promising material for infrared diode lasers and detectors in the wavelength region between 6 and 30 micron. Since the electrical properties of Pb(1-x)Sn(x)Te depend greatly on the Pb/Sn ratio and crystalline defects as well as impurity concentration, homogeneous, defect-free, high-quality crystals are anticipated. Although many growth methods, such as the pulling method, the Bridgman method, the vapor growth method, etc., have been applied to the growth of Pb(1-x)Sn(x)Te, large, homogeneous, low-defect-density crystals have not yet been grown on Earth. The unsuccessful results were caused by buoyancy-driven convection in the fluids induced by the specific gravity difference between heated and cooled fluids on Earth. A crystal is grown by cooling the melt from one end of the ampoule. In crystal growth from the melt, about 30 percent of the SnTe in the melt is rejected at the solid-liquid interface during solidification. On Earth, the rejected SnTe is completely mixed with the remaining melt by convection in the melt. Therefore, SnTe concentration in the melt, and accordingly in the crystal, increases as the crystal grows. In the microgravity environment, buoyancy-driven convection is suppressed because the specific gravity difference is negligible. In that case, the rejected SnTe remains at the solid-liquid interface and its concentration increases only at the interface. If the growth rate is higher than the PbTe-SnTe interdiffusion rate, the amount of SnTe which diffuses from the interface into the melt increases as SnTe piles up at the interface, and finally it balances the amount of rejected SnTe during solidification, resulting in steady-state SnTe transportation at the interface. By using this principle, compositionally homogeneous crystals can be grown. Furthermore, low-defect-density crystals will be grown in microgravity, because convection causes crystalline defects by mising hot and cold fluids and generating temperature fluctuations in them.

Post-Growth Annealing of Bridgman-grown CdZnTe and CdMnTe Crystals for Room-temperature Nuclear Radiation Detectors

DOE PAGES

Egarievwe, Stephen U.; Yang, Ge; Egarievwe, Alexander; ...

2015-02-11

Bridgman-grown cadmium zinc telluride (CdZnTe or CZT) and cadmium manganese telluride (CdMnTe or CMT) crystals often have Te inclusions that limit their performances as X-ray- and gamma-ray-detectors. We present here the results of post-growth thermal annealing aimed at reducing and eliminating Te inclusions in them. In a 2D analysis, we observed that the sizes of the Te inclusions declined to 92% during a 60-h annealing of CZT at 510 °C under Cd vapor. Further, tellurium inclusions were eliminated completely in CMT samples annealed at 570 °C in Cd vapor for 26 h, whilst their electrical resistivity fell by an ordermore » of 10 2. During the temperature-gradient annealing of CMT at 730 °C and an 18 °C/cm temperature gradient for 18 h in a vacuum of 10 -5 mbar, we observed the diffusion of Te from the sample, causing a reduction in size of the Te inclusions. For CZT samples annealed at 700 °C in a 10 °C/cm temperature gradient, we observed the migration of Te inclusions from a low-temperature region to a high one at 0.022 μm/s. During the temperature-gradient annealing of CZT in a vacuum of 10 -5 mbar at 570 °C and 30 °C/cm for 18 h, some Te inclusions moved toward the high-temperature side of the wafer, while other inclusions of the same size, i.e., 10 µm in diameter, remained in the same position. These results show that the migration, diffusion, and reaction of Te with Cd in the matrix of CZT- and CMT-wafers are complex phenomena that depend on certain conditions.« less

Heat transfer simulation in a vertical Bridgman CdTe growth configuration

NASA Astrophysics Data System (ADS)

Martinez-Tomas, C.; Muñoz, V.; Triboulet, R.

1999-02-01

Modelling and numerical simulation of crystal growth processes have been shown to be powerful tools in order to understand the physical effects of different parameters on the growth conditions. In this study a finite difference/control volume technique for the study of heat transfer has been employed. This model takes into account the whole system: furnace temperature profile, air gap between furnace walls and ampoule, ampoule geometry, crucible coating if any, solid and liquid CdTe thermal properties, conduction, convection and radiation of heat and phase change. We have used the commercial code FLUENT for the numerical resolution that can be running on a personal computer. Results show that the temperature field is very sensitive to the charge and ampoule peculiarities. As a consequence, significant differences between the velocity of the ampoule and that of the isotherm determining the solid/liquid interface have been found at the onset of the growth.

Crystal structure and thermal expansion of a CsCe 2Cl 7 scintillator

DOE PAGES

Zhuravleva, M.; Lindsey, A.; Chakoumakos, B. C.; ...

2015-04-06

Here we used single-crystal X-ray diffraction data to determine crystal structure of CsCe 2Cl 7. It crystallizes in a P112 1/b space group with a = 19.352(1) Å, b = 19.352(1) Å, c = 14.838(1) Å, γ = 119.87(2) ° , and V = 4818.6(5) Å 3. Differential scanning calorimetry measurements combined with the structural evolution of CsCe 2Cl 7 via X-ray diffractometry over a temperature range from room temperature to the melting point indicates no obvious intermediate solid-solid phase transitions. The anisotropy in the average linear coefficient of thermal expansion of the a axis (21.3 10 -6/ °C) withmore » respect to the b and c axes (27.0 10 -6/ °C) was determined through lattice parameter refinement of the temperature dependent diffraction patterns. Lastly, these findings suggest that the reported cracking behavior during melt growth of CsCe 2Cl 7 bulk crystals using conventional Bridgman and Czochralski techniques may be largely attributed to the anisotropy in thermal expansion.« less

Design and growth of novel compounds for radiation sensors: multinary chalcogenides

NASA Astrophysics Data System (ADS)

Singh, N. B.; Su, Ching-Hua; Nagaradona, Teja; Arnold, Brad; Choa, Fow-Sen

2016-05-01

Increasing threats of radiological weapons have revitalized the researches for low cost large volume γ-ray and neutron ray sensors In the past few years we have designed and grown ternary and quaternary lead and thallium chalcogenides and lead selenoiodides for detectors to meet these challenges. These materials are congruent, can be tailored to enhance the parameters required for radiation sensors. In addition, this class of compounds can be grown by Bridgman method which promises for large volume productions. We have single crystals of several compounds from the melt including Tl3AsSe3, Tl3AsSe3-xSx, TlGaSe2, AgGaGe3Se8, AgxLi1-xAgGaGe3Se8 and PbTlI5-x Sex compounds. Experimental studies indicate that these have very low absorption coefficient, low defect density and can be fabricated in any shape and sizes. These crystals do not require post growth annealing and do not show any second phase precipitates when processed for electrode bonding and other fabrication steps. In this paper we report purification, growth and fabrication of large Tl3AsSe3 (TAS) crystals. We observed that TAS crystals grown by using further purification of as supplied high purity source materials followed by directionally solidified charge showed higher resistivity than previously reported values. TAS also showed constant value as the function of voltage.

Numerical Modeling of Solidification in Space With MEPHISTO-4. Part 2

NASA Technical Reports Server (NTRS)

Simpson, James E.; Yoa, Minwu; deGroh, Henry C., III; Garimella, V. Suresh

1998-01-01

A pre-flight analysis of the directional solidification of BiSn with MEPHISTO-4 is presented. Simplified Bridgman growth under microgravity conditions is simulated using a two dimensional finite element model. This numerical model is a single domain, pseudo-steady state model, and includes the effects of both thermal and solutal convection. The results show that for all orientations of the applied steady state gravity vector, of magnitude 1 micro-g, the directional solidification process remains diffusion controlled. The maximum convective velocity was found to be 4.424 x 10(exp -5) cm/s for the horizontal Bridgman growth configuration. This value is an order of magnitude lower than the growth velocity. The maximum and minimum values or solute concentration in the liquid at the crystal-melt interface were 13.867 at.% and 13.722 at.%, respectively. This gives a radial segregation value of xi = 1.046% at the interface. A secondary objective of this work was to compare the results obtained to those that consider thermal convection only (no solutal convection). It was found that the convective flow patterns in simulations which included solutal convection were significantly different from those which ignored solutal convection. The level of radial segregation predicted by the current simulations is an order of magnitude lower than that found in simulations which ignore solutal convection. The final aim was to investigate the effect of g-jitter on the crystal growth process. A simulation was performed to calculate the system response to a 1 second, 100 micro-g gravity impulse acting normal to the direction of growth. This pulse is consistent with that induced by Orbiter thruster firings. The results obtained indicate that such a gravity pulse causes an increase in the level of radial solute segregation at the interface from the steady state values. The maximum value of solute concentration in the liquid was found to be 13.888 at.%, the minimum value calculated was 13.706 at.%, yielding a radial segregation value of xi = 1.31% at the interface. These values occurred 126 seconds after the pulse terminated. Thus it is anticipated that the process will remain diffusion controlled even when subjected to such g-jitter.

Exploring growth conditions and Eu2+ concentration effects for KSr2I5:Eu scintillator crystals

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Camarda, G.; Lindsey, A.; Johnson, J.; Hobbs, C.; Melcher, C. L.

2016-04-01

Our current research is focused on understanding dopant optimization, growth rate, homogeneity and their impact on the overall performance of KSr2I5:Eu2+ single crystal scintillators. In this work we have investigated the effects of Eu2+ concentration in the potassium strontium iodide matrix, and we found that the concentration needed to maximize the light yield was 4 mol%. In order to assess the effects of the pulling rate, we grew single crystals at 12, 24 and 120 mm/day via the vertical Bridgman technique. For the sample sizes measured (5×5×5 mm3), we found that the crystal grown at the fastest rate of 120 mm/day showed a light yield within ~7% of the more slowly grown boules, and no significant change was observed in the energy resolution. Therefore, light yields from 88,000 to 96,000 ph/MeV and energy resolutions from 2.4 to 3.0% (at 662 keV) were measured for KSr2I5:Eu 4% over a relatively wide range of growth conditions. In order to assess the homogeneity of KSr2I5:Eu 4%, a newly developed micro-resolution X-ray technique was used to map the light yield as a function of excitation position. In the crystals that we studied, we did not observe any significant inhomogeneity other than a smooth gradient due to light collection and self absorption effects.

Directional growth and characterization of Fe?Al?Nb eutectic alloys

NASA Astrophysics Data System (ADS)

Mota, M. A.; Coelho, A. A.; Bejarano, J. M. Z.; Gama, S.; Caram, R.

1999-03-01

The manufacturing of components for operation at high temperatures requires the use of metallic materials which can keep satisfactory mechanical and chemical properties, even at temperatures beyond 1000°C. An interesting alternative to solve such a problem is the use of directionally solidified eutectic alloys. A potentially promising system for the manufacture of structural materials, and so far not totally studied, is the eutectic based on the Fe-Al-Nb system, which involves the (FeAl) 2Nb phase and the FeAl solid solution. Eutectic samples from this system were directionally solidified in a vertical Bridgman crystal growth unit. The objective of the experiments was to determine the influence of the growth rate on the eutectic microstructure. The ingots obtained were investigated by using optical and electron scanning microscopy. At low growth rate, the eutectic microstructure remained regular, even though it showed several types of microstructure defects. As the growth rate was increased, a transition from lamellar to fibrous morphology was observed.

Testing and Further Development of Improved Etches and Etching Methods for the Analysis of Bridgman Grown Semiconductor Crystals with an Emphasis on Lead-Tin-Telluride

NASA Technical Reports Server (NTRS)

Barber, Patrick G.

1998-01-01

The goals outlined for the research project for this year have been completed, and the following supporting documentation is attached: 1. A copy of the proposal outlining the principal goals: (a) Improve the characterization of semiconductor crystals through new etches and etching procedures. (b) Developed a novel voltammetric method to characterize semiconductor crystals as a result of searching for improved etches for lead-tin-telluride. (c) Presented paper at ACCG- 10. (d) Prepared manuscripts for publication. Completed additional testing suggested by reviewers and re-submitted manuscripts. (e) Worked with an undergraduate student on this project to provide her an opportunity to have a significant research experience prior to graduation. 2. In addition to the anticipated goals the following were also accomplished: (a) Submitted the newly developed procedures for consideration as a patent or a NASA Tech Brief. (b) Submitted a paper for presentation at the forthcoming ICCG- 12 conference. 3. A copy of the final draft of the publication as submitted to the editors of the Journal of Crystal Growth.

Kinetics of the current response in TlBr detectors under a high dose rate of {gamma}-ray irradiation

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

Gazizov, I. M., E-mail: gazizov@isotop.dubna.ru; Zaletin, V. M.; Kukushkin, V. M.

2012-03-15

The kinetics of the photocurrent response in doped and undoped TlBr samples subjected to irradiation with {gamma}-ray photons from a {sup 137}Cs source with the dose rate 0.033 to 3.84 Gy/min are studied. The crystals were grown by the directional crystallization of the melt method using the Bridgman-Stockbarger technique. The Pb impurity mass fraction introduced into the doped TlBr crystals was 1-10 ppm and amounted to 150 ppm for the Ca impurity. The crystals were grown in a vacuum, in bromine vapors, in a hydrogen atmosphere, and in air. Decay of the photocurrent is observed for extrinsic semiconductor crystals dopedmore » with bivalent cations (irrespective of the growth atmosphere), and also for crystals grown in hydrogen and crystals grown in an excess of thallium. The time constant of photocurrent decay {tau} amounted to 30-1400 s and was proportional to resistivity. It is shown that the current response can be related to photolysis in the TlBr crystals during irradiation with {gamma}-ray photons. The energy of hole traps responsible for a slow increase in the photo-current has been estimated and found to be equal to 0.6-0.85 eV.« less

Anisotropy of the Mechanical Properties of TbF3 Crystals

NASA Astrophysics Data System (ADS)

Karimov, D. N.; Lisovenko, D. S.; Sizova, N. L.; Sobolev, B. P.

2018-01-01

TbF3 (sp. gr. Pnma) crystals up to 40 mm in diameter have been grown from melt by a Bridgman technique. The anisotropy of their mechanical properties is studied for the first time. the technical elasticity constants are calculated, and room-temperature values of Vickers microhardness for the (010) and (100) planes are measured. The shape of indentation impressions is found to correlate with Young's modulus anisotropy for TbF3 crystals.

A Numerical Investigation of the Effect of Thermoelectromagnetic Convection (TEMC) on the Bridgman Growth of Ge(1-x)Si(x)

NASA Technical Reports Server (NTRS)

Yesilyurt, Serhat; Vujisic, Ljubomir; Motakef, Shariar; Szofran, F. R.; Volz, Martin P.

1998-01-01

Thermoelectric currents at the growth interface of GeSi during Bridgman growth are shown to promote convection when a low intensity axial magnetic field is applied. TEMC, typically, is characterized by a meridional flow driven by the rotation of the fluid; meridional convection alters composition of the melt, and shape of the growth interface substantially. TEMC effect is more important in micro-gravity environment than the terrestrial one, and can be used to control convection during the growth of GeSi. In this work, coupled thermo-solutal flow equations (energy, scalar transport, momentum and mass) are solved in tandem with Maxwell's equations to compute the thermo-solutat flow field, electric currents, and the growth-interface shape.

Defect Engineering in SrI 2:Eu 2+ Single Crystal Scintillators

DOE PAGES

Wu, Yuntao; Boatner, Lynn A.; Lindsey, Adam C.; ...

2015-06-23

Eu 2+-activated strontium iodide is an excellent single crystal scintillator used for gamma-ray detection and significant effort is currently focused on the development of large-scale crystal growth techniques. A new approach of molten-salt pumping or so-called melt aging was recently applied to optimize the crystal quality and scintillation performance. Nevertheless, a detailed understanding of the underlying mechanism of this technique is still lacking. The main purpose of this paper is to conduct an in-depth study of the interplay between microstructure, trap centers and scintillation efficiency after melt aging treatment. Three SrI 2:2 mol% Eu2+ single crystals with 16 mm diametermore » were grown using the Bridgman method under identical growth conditions with the exception of the melt aging time (e.g. 0, 24 and 72 hours). Using energy-dispersive X-ray spectroscopy, it is found that the matrix composition of the finished crystal after melt aging treatment approaches the stoichiometric composition. The mechanism responsible for the formation of secondary phase inclusions in melt-aged SrI 2:Eu 2+ is discussed. Simultaneous improvement in light yield, energy resolution, scintillation decay-time and afterglow is achieved in melt-aged SrI 2:Eu 2+. The correlation between performance improvement and defect structure is addressed. The results of this paper lead to a better understanding of the effects of defect engineering in control and optimization of metal halide scintillators using the melt aging technique.« less

Surface defect free growth of a spin dimer TlCuCl{sub 3} compound crystals and investigations on its optical and magnetic properties

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

Ryu, Gihun, E-mail: G.Ryu@fkf.mpg.de; Son, Kwanghyo

A defect-free high quality single crystal of spin dimer TlCuCl{sub 3} compound is firstly synthesized at the optimal growth temperature using the vertical Bridgman method. In this study, we clearly found that the cupric chloride is easily decomposed into the Cl{sup −} deficient composition at ≥470 °C. The Cl{sup −}- related gas phase at the high temperature region also always gives rise to a pinhole-like surface defect at the surface of crystal. Therefore, we clearly verified an exotic anisotropic magnetic behavior (anisotropic ratio of M{sub b}/M{sub (201)} at 2 K, 7 T=10) using the defect-free TlCuCl{sub 3} crystals in thismore » three-dimensional spin dimer TlCuCl{sub 3} compound, relatively stronger magnetic ordering in the H//b than that of H//(201) direction at above the transition magnetic field. - Graphical abstract: A single crystal of spin dimer TlCuCl{sub 3} compound with a defect free is successfully synthesized on the basis of TG/DTA result. We newly found that this cupric chloride compound is easily decomposed into the Cl{sup −} deficient composition at ≥470 °C and Cl{sup −} related gas phases also give rise to the defects like a pinhole on the surface of TlCuCl{sub 3} crystal. Using the crystals with a surface defect free, we also clearly verified the crystal structure of spin dimer TlCuCl{sub 3} compound.« less

Crystal growth and scintillation properties of strontium iodide scintillators

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

van Loef, Edgar; Wilson, Cody; Cherepy, Nerine

2009-06-01

Single crystals of SrI{sub 2}:Eu and SrI{sub 2}:Ce/Na were grown from anhydrous iodides by the vertical Bridgman technique in evacuated silica ampoules. Growth rates were of the order of 5-30 mm/day. Radioluminescence spectra of SrI{sub 2}:Eu and SrI{sub 2}:Ce/Na exhibit a broad band due to Eu{sup 2+} and Ce{sup 3+} emission, respectively. The maximum in the luminescence spectrum of SrI{sub 2}:Eu is found at 435 nm. The spectrum of SrI{sub 2}:Ce/Na exhibits a doublet peaking at 404 and 435 nm attributed to Ce{sup 3+} emission, while additional impurity - or defected - related emission is present at approximately 525 nm.more » The strontium iodide scintillators show very high light yields of up to 120,000 photons/MeV, have energy resolutions down to 3% at 662 keV (Full Width Half Maximum) and exhibit excellent light yield proportionality with a standard deviation of less than 5% between 6 and 460 keV.« less

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

NASA Technical Reports Server (NTRS)

Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

1999-01-01

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Growth of congruently melting Ca0.59Sr0.41F2 crystals and study of their properties

NASA Astrophysics Data System (ADS)

Karimov, D. N.; Komar'kova, O. N.; Sorokin, N. I.; Bezhanov, V. A.; Chernov, S. P.; Popov, P. A.; Sobolev, B. P.

2010-05-01

Homogeneous crystals of Ca0.59Sr0.41F2 alloy (sp. gr., Fm bar 3 m, a = 0.56057 nm), corresponding to the point of minimum in the melting curve in the CaF2-SrF2 phase diagram, have been grown by the vertical Bridgman method. The optical, mechanical, electrical, and thermophysical properties of Ca0.59Sr0.41F2 and MF2 crystals ( M = Ca, Sr) have been studied and comparatively analyzed. Ca0.59Sr0.41F2 crystals are transparent in the range of 0.133-11.5 μm, have refractive index n D = 1.436, microhardness H μ = 2.63 ± 0.10 GPa, ion conductivity σ = 5 × 10-5 S/cm at 825 K, and thermal conductivity k = 4.0 W m-1 K-1 at 300 K. It is shown that the optical properties of Ca0.59Sr0.41F2 crystals are intermediate between those of CaF2 and SrF2, whereas their mechanical and electrical characteristics are better than the latter compounds.

Characterization of the intrinsic scintillator Cs 2LiCeCl 6

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

James, R.

2017-10-02

In this work, we report on the scintillation properties of the intrinsic scintillator Cs 2LiCeCl 6 (CLCC), which is potentially useful for dual gamma-ray and neutron detection. CLCC is from the elpasolite family with a cubic structure. We grew the crystals at BNL by the vertical Bridgman growth technique. The luminescence spectrum of CLCC showed a doublet with peak maxima at 384 nm and 402 nm. The light yield of CLCC was approximately 20,000 photons/MeV, and the energy resolution was about 6% for 662-keV gamma radiation. A scintillation decay of ~81% of the total light was observed to be ~more » 90 nanoseconds.« less

Proceedings of Symposium F on New Aspects on the Growth, Characterization and Applications of CdTe and Related Cd Rich Alloys of the 1992 E-MRS Spring Conference held in Strasbourg, France on June 2 - 5, 1992

DTIC Science & Technology

1992-01-01

Bridgman method VI - with (VBZ) and without (VB) a cadmium source can be 1- observed. In VB crystals grown from a slightly tellurium-rich melt the axial...CdTe epilayers will be performed ex 3. Results situ. Light sources are, respectively, a low power HeNe laser emitting at 633 nm and a 75 W xenon lamp for...Positrons can be used as a probe of vacancy-type recorded about 2 x 106 annihilations. After source and defects in semiconductors by studying their

Charge transport properties in CdZnTe detectors grown by the vertical Bridgman technique

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

Auricchio, N.; Caroli, E.; Marchini, L.

2011-12-15

Presently, a great amount of effort is being devoted to the development of CdTe and CdZnTe (CZT) detectors for a large variety of applications such as medical, industrial, and space research. We present the spectroscopic properties of some CZT crystals grown by the standard vertical Bridgman method and by the boron oxide encapsulated vertical Bridgman method, which has been recently implemented at IMEM-CNR (Parma, Italy). In this technique, the crystal is grown in an open quartz crucible fully encapsulated by a thin layer of liquid boron oxide. This method prevents contact between the crystal and the crucible, thereby allowing largermore » single grains with a lower dislocation density to be obtained. Several mono-electrode detectors were realized, with each having two planar gold contacts. The samples are characterized by an active area of about 7 mm x 7 mm and thicknesses ranging from 1 to 2 mm. The charge transport properties of the detectors have been studied by mobility-lifetime ({mu} x {tau}) product measurements, carried out at the European Synchrotron Radiation Facility (Grenoble, France) in the planar transverse field configuration, where the impinging beam direction is orthogonal to the collecting electric field. We have performed several fine scans between the electrodes with a beam spot of 10 {mu}m x 10 {mu}m at various energies from 60 to 400 keV. In this work, we present the test results in terms of the ({mu} x {tau}) product of both charge carriers.« less

Growth and characterization of binary and pseudo-binary 3-5 compounds exhibiting non-linear optical behavior. Undergraduate research opportunities in microgravity science and technology

NASA Technical Reports Server (NTRS)

Witt, August F.

1992-01-01

In line with the specified objectives, a Bridgman-type growth configuration in which unavoidable end effects - conventionally leading to growth interface relocation - are compensated by commensurate input-power changes is developed; the growth rate on a microscale is predictable and unaffected by changes in heat transfer conditions. To permit quantitative characterization of the growth furnace cavity (hot-zone), a 3-D thermal field mapping technique, based on the thermal image, is being tested for temperatures up to 1100 C. Computational NIR absorption analysis was modified to now permit characterization of semi-insulating single crystals. Work on growth and characterization of bismuth-silicate was initiated. Growth of BSO (B12SiO20) for seed material by the Czochralski technique is currently in progress. Undergraduate research currently in progress includes: ground based measurements of the wetting behavior (contact angles) of semiconductor melts on substrates consisting of potential confinement materials for solidification experiments in a reduced gravity environment. Hardware modifications required for execution of the wetting experiments in a KC-135 facility are developed.

p-type doping efficiency in CdTe: Influence of second phase formation

NASA Astrophysics Data System (ADS)

McCoy, Jedidiah J.; Swain, Santosh K.; Sieber, John R.; Diercks, David R.; Gorman, Brian P.; Lynn, Kelvin G.

2018-04-01

Cadmium telluride (CdTe) high purity, bulk, crystal ingots doped with phosphorus were grown by the vertical Bridgman melt growth technique to understand and improve dopant solubility and activation. Large net carrier densities have been reproducibly obtained from as-grown ingots, indicating successful incorporation of dopants into the lattice. However, net carrier density values are orders of magnitude lower than the solubility of P in CdTe as reported in literature, 1018/cm3 to 1019/cm3 [J. H. Greenberg, J. Cryst. Growth 161, 1-11 (1996) and R. B. Hall and H. H. Woodbury, J. Appl. Phys. 39(12), 5361-5365 (1968)], despite comparable starting charge dopant densities. Growth conditions, such as melt stoichiometry and post growth cooling, are shown to have significant impacts on dopant solubility. This study demonstrates that a significant portion of the dopant becomes incorporated into second phase defects as compounds of cadmium and phosphorous, such as cadmium phosphide, which inhibits dopant incorporation into the lattice and limits maximum attainable net carrier density in bulk crystals. Here, we present an extensive study on the characteristics of these second phase defects in relation to their composition and formation kinetics while providing a pathway to minimize their formation and enhance solubility.

The effects of Peltier marking on semiconductor growth in a magnetic field

NASA Astrophysics Data System (ADS)

Sellers, Cheryl Casper

This research represents a model for three dimensional semiconductor growth in a vertical Bridgman process within an externally applied magnetic field with the additional effects of Peltier marking. The magnetic field is strong enough that inertial effects can be neglected and that viscous effects are confined to boundary layers. The objective of this research is a first step in the development of a method to accurately predict the distribution of dopants and species in the melt after a current pulse with a given duration and strength, with a given magnetic field and with a given crystal-melt interface shape. The first model involves an asymptotic solution to provide physical clarification of the flow. In both models the crystal/melt interface is modeled as fr=3r2 where 3≪1 . The first model incorporates a variable, a which ranges from 0.25 to 1.0. The second model involves an analytical solution with an arbitrary Ha and a≪1 . These models show the how the azimuthal velocity varies with increasing Ha and how the stream function varies in the meridional problem. This gives insight into how the dopant is mixed during the crystal growth process. The results demonstrate that current pulses with relatively weak magnetic fields and modest interface curvature can lead to very strong mixing in the melt.

Photoconductivity in the chalcohalide semiconductor, SbSeI: a new candidate for hard radiation detection.

PubMed

Wibowo, Arief C; Malliakas, Christos D; Liu, Zhifu; Peters, John A; Sebastian, Maria; Chung, Duck Young; Wessels, Bruce W; Kanatzidis, Mercouri G

2013-06-17

We investigated an antimony chalcohalide compound, SbSeI, as a potential semiconductor material for X-ray and γ-ray detection. SbSeI has a wide band gap of 1.70 eV with a density of 5.80 g/cm(3), and it crystallizes in the orthorhombic Pnma space group with a one-dimensional chain structure comprised of infinite zigzag chains of dimers [Sb2Se4I8]n running along the crystallographic b axis. In this study, we investigate conditions for vertical Bridgman crystal growth using combinations of the peak temperature and temperature gradients as well as translation rate set in a three-zone furnace. SbSeI samples grown at 495 °C peak temperature and 19 °C/cm temperature gradient with 2.5 mm/h translation rate produced a single phase of columnar needlelike crystals aligned along the translational direction of the growth. The ingot sample exhibited an n-type semiconductor with resistivity of ∼10(8) Ω·cm. Photoconductivity measurements on these specimens allowed us to determine mobility-lifetime (μτ) products for electron and hole carriers that were found to be of similar order of magnitude (∼10(-4) cm(2)/V). Further, the SbSeI ingot with well-aligned, one-dimensional columnar needlelike crystals shows an appreciable response of Ag Kα X-ray.

Characteristics of a promising new thermoelectric material - Ruthenium silicide

NASA Technical Reports Server (NTRS)

Ohta, Toshitaka; Vining, Cronin B.; Allevato, Camillo E.

1991-01-01

A preliminary study on arc-melted samples has indicated that ruthenium silicide has the potential to obtain figure-of-merit values four times higher than that of conventional silicon-germanium material. In order to realize the high figure-of-merit values, high-quality crystal from the melt is needed. A Bridgman-like method has been employed and has realized much better crystals than arc-melted ones.

Simulation of radial solute segregation in vertical Bridgman growth of pyridine-doped benzene, a surrogate for binary organic nonlinear optical materials

NASA Astrophysics Data System (ADS)

Lee, Hanjie; Pearlstein, Arne J.

2000-09-01

We present steady axisymmetric computations of solute distributions and radial segregation for vertical Bridgman growth of pyridine-doped benzene, a binary aromatic system with anisotropic solid-phase thermal conductivity, that serves as a model of solute transport in crystal growth of organic nonlinear optical materials. The radial variation of solid-phase mass fraction ( Cs) of pyridine, which is rejected at the growing interface, depends strongly on growth conditions. High growth velocities tend to increase Cs near the centerline, the ampoule wall, or both, and low growth velocities give more nearly uniform radial distributions. The maximum ampoule-wall temperature gradient also affects radial segregation, with convex-to-the-liquid interfaces at small temperature gradients being associated with radially monotonic Cs distributions, and ridged interfaces at higher gradients being associated with nonmonotonic distributions having maxima at the centerline and ampoule wall. Nonuniformity is strongly determined by both interface shape and the nature of the flow near the interface. Solute is transported down to the interface by a large toroidal vortex, and swept radially inward to the centerline by a second, flattened toroidal cell. When the interface is depressed at its junction with the ampoule wall, rejected solute accumulates in the overlying liquid, where convection is relatively weak, resulting in local solute enrichment of the solid. Computations at normal and zero gravity show that for two very similar interface shapes, a maximum in the radial solid-phase solute distribution at the ampoule wall is associated with the interface shape, while the maximum on the centerline is associated with sweeping of solute to the centerline by a vortical flow on the interface. We also show that radial solute segregation depends significantly on whether account is taken of the anisotropy of the solid-phase thermal conductivity. Finally, the computations provide guidance as to the minimum ampoule length required to produce an axially uniform solute distribution over at least part of the length of a boule.

On the scaling analysis of the solute boundary layer in idealized growth configurations

NASA Astrophysics Data System (ADS)

Garandet, J. P.; Duffar, T.; Favier, J. J.

1990-11-01

A scaling procedure is applied to the equation governing chemical transport in idealized Czochralski and horizontal Bridgman growth experiments. Our purpose is to get a fair estimate of the solute boundary layer in front of the solidification interface. The results are very good in the Czochralski type configuration, the maximum error with respect to the semi-analytical solution of Burton, Prim and Schlichter being of the order of 20%. In the Bridgman type configuration, our predictions compare well with the values of the numerical simulations; however, more data would be needed for a definite conclusion to be drawn.

Laser ultrasonic investigations of vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Queheillalt, Douglas Ted

The many difficulties associated with the growth of premium quality CdTe and (Cd,Zn)Te alloys has stimulated an interest in the development of a non-invasive ultrasonic approach to monitor critical growth parameters such as the solid-liquid interface position and shape during vertical Bridgman growth. This sensor methodology is based upon the recognition that in most materials, the ultrasonic velocity (and the elastic stiffness constants that control it) of the solid and liquid phases are temperature dependent and an abrupt increase of the longitudinal wave velocity occurs upon solidification. The laser ultrasonic approach has also been used to measure the ultrasonic velocity of solid and liquid Cd0.96Zn0.04Te as a function of temperature up to 1140°C. Using longitudinal and shear wave velocity values together with data for the temperature dependent density allowed a complete evaluation of the temperature dependent single crystal elastic stiffness constants for solid and the adiabatic bulk modulus for liquid Cd0.96Zn0.04 Te. It was found that the ultrasonic velocities exhibited a strong monotonically decreasing function of temperature in the solid and liquid phases and the longitudinal wave indicated an abrupt almost 50% decrease upon melting. Because ray propagation in partially solidified bodies is complex and defines the sensing methodology, a ray tracing algorithm has been developed to analyze two-dimensional wave propagation in the diametral plane of cylindrical solid-liquid interfaces. Ray path, wavefront and time-of-flight (TOF) projections for rays that travel from a source to an arbitrarily positioned receiver on the diametral plane have been calculated and compared to experimentally measured data on a model liquid-solid interface. The simulations and the experimental results reveal that the interfacial region can be identified from transmission TOF data and when used in conjunction with a nonlinear least squares reconstruction algorithm, the interface geometry (i.e. axial location and shape) can be precisely recovered and the ultrasonic velocities of both solid and liquid phases obtained. To gain insight into the melting and solidification process, a single zone VB growth furnace was integrated with the laser ultrasonic sensor system and used to monitor the melting-solidification and directional solidification characteristics of Cd0.96Zn 0.04Te.

Tl{sub 10}Hg{sub 3}Cl{sub 16}: Single crystal growth, electronic structure and piezoelectric properties

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

Khyzhun, O.Y., E-mail: khyzhun@ipms.kiev.ua; Piasecki, M.; Kityk, I.V.

Single crystal of the ternary halide Tl{sub 10}Hg{sub 3}Cl{sub 16} was grown using Bridgman-Stockbarger method. For the Tl{sub 10}Hg{sub 3}Cl{sub 16} crystal, we have measured X-ray photoelectron spectra for both pristine and Ar{sup +} ion-bombarded surfaces and additionally investigated photoinduced piezoelectricity. Our data indicate that the Tl{sub 10}Hg{sub 3}Cl{sub 16} single crystal surface is very sensitive with respect to Ar{sup +} ion-bombardment. In particular, Ar{sup +} ion-bombardment with energy of 3.0 keV over 5 min at an ion current density of 14 μA/cm{sup 2} causes significant changes of the elemental stoichiometry of the Tl{sub 10}Hg{sub 3}Cl{sub 16} surface resulting inmore » an abrupt decrease of the mercury content in the top surface layers of the studied single crystal. As a result of the treatment, the mercury content becomes nil in the top surface layers. In addition, the present XPS measurements allow for concluding about very low hygroscopicity of the Tl{sub 10}Hg{sub 3}Cl{sub 16} single crystal surface. The property is extremely important for the crystal handling in optoelectronic or nano-electronic devices working at ambient conditions. The photoinduced piezoelectricity has been explored for Tl{sub 10}Hg{sub 3}Cl{sub 16} depending on nitrogen (λ=371 nm) laser power density and temperature. - Graphical abstract: As-grown single crystal boule of Tl{sub 10}Hg{sub 3}Cl{sub 16}; dependence of the effective piezoelecric coefficient d{sub 33} versus the photoinducing nitrogen laser power density, I, at different temperatures, T; and packing of the polyhedra of halide atoms around Hg atoms in the Tl{sub 10}Hg{sub 3}Cl{sub 16} structure. - Highlights: • High-quality Tl{sub 10}Hg{sub 3}Cl{sub 16} single crystal has been grown by Bridgman-Stockbarger method. • Electronic structure of Tl{sub 10}Hg{sub 3}Cl{sub 16} is studied by the XPS method. • Tl{sub 10}Hg{sub 3}Cl{sub 16} single crystal surface is sensitive with respect to Ar{sup +} ion-bombardment. • Very low hygroscopicity is characteristic of the Tl{sub 10}Hg{sub 3}Cl{sub 16} surface. • Photoinduced piezoelectricity is studied for the Tl{sub 10}Hg{sub 3}Cl{sub 16} compound.« less

Post-growth annealing of Bridgman-grown CdZnTe and CdMnTe crystals for room-temperature nuclear radiation detectors

NASA Astrophysics Data System (ADS)

Egarievwe, Stephen U.; Yang, Ge; Egarievwe, Alexander A.; Okwechime, Ifechukwude O.; Gray, Justin; Hales, Zaveon M.; Hossain, Anwar; Camarda, Giuseppe S.; Bolotnikov, Aleksey E.; James, Ralph B.

2015-06-01

Bridgman-grown cadmium zinc telluride (CdZnTe or CZT) and cadmium manganese telluride (CdMnTe or CMT) crystals often have Te inclusions that limit their performances as X-ray- and gamma-ray-detectors. We present here the results of post-growth thermal annealing aimed at reducing and eliminating Te inclusions in them. In a 2D analysis, we observed that the sizes of the Te inclusions declined to 92% during a 60-h annealing of CZT at 510 °C under Cd vapor. Further, tellurium inclusions were eliminated completely in CMT samples annealed at 570 °C in Cd vapor for 26 h, whilst their electrical resistivity fell by an order of 102. During the temperature-gradient annealing of CMT at 730 °C and an 18 °C/cm temperature gradient for 18 h in a vacuum of 10-5 mbar, we observed the diffusion of Te from the sample, so causing a reduction in size of the Te inclusions. For CZT samples annealed at 700 °C in a 10 °C/cm temperature gradient, we observed the migration of Te inclusions from a low-temperature region to a high one at 0.022 μm/s. During the temperature-gradient annealing of CZT in a vacuum of 10-5 mbar at 570 °C and 30 °C/cm for 18 h, some Te inclusions moved toward the high-temperature side of the wafer, while other inclusions of the same size, i.e., 10 μm in diameter, remained in the same position. These results show that the migration, diffusion, and reaction of Te with Cd in the matrix of CZT- and CMT-wafers are complex phenomena that depend on the conditions in local regions, such as composition and structure, as well as on the annealing conditions.

Control of Meridional Flow by a Non-Uniform Rotational Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Ramachandran, Narayanan

1999-01-01

The diffusive mass transfer of species during crystal growth in vertical ampoules is significantly affected by fluid flow in the liquid mother phase (melt). For electrically conductive melts, an elegant way of remotely inducing and controlling this flow is by utilizing a uniform rotational magnetic field (RMF) in the transverse direction. It induces an azimuthal flow which tends to homogenize the thermal and solutal fields. The rotating field also reduces the diffusion boundary layer, stabilizes temperature fluctuations, and promotes better overall crystal growth. For moderate strengths of the applied magnetic field (2-20 m Tesla) with frequencies of up to 400 Hz, the induced secondary meridional flow becomes significant. It typically consists of one roll at the bottom of the liquid column and a second roll (vortex) at the top. The flow along the centerline (ampoule axis) is directed from the growing solid (interface) towards the liquid (melt). In case of convex interfaces (e.g. in floating zone crystal growth) such flow behavior is beneficial since it suppresses diffusion at the center. However, for concave interfaces (e.g. vertical Bridgman crystal growth) such a flow tends to exacerbate the situation in making the interface shape more concave. It would be beneficial to have some control of this meridional flow- for example, a single recirculating cell with controllable direction and flow magnitude will make this technique even more attractive for crystal growth. Such flow control is a possibility if a non-uniform PNE field is utilized for this purpose. Although this idea has been proposed earlier, it has not been conclusively demonstrated so far. In this work, we derive the governing equations for the fluid dynamics for such a system and obtain solutions for a few important cases. Results from parallel experimental measurements of fluid flow in a mercury column subjected to non-uniform RMF will also be presented.

Improved lithium iodide neutron scintillator with Eu 2+ activation: The elimination of Suzuki-Phase precipitates

DOE PAGES

Boatner, Lynn A.; Comer, Eleanor P.; Wright, Gomez W.; ...

2017-02-21

Monovalent alkali halides such as NaI, CsI, and LiI are widely used as inorganic scintillators for radiation detection due to their light yield, the capability for the growth of large single crystals, relatively low cost, and other favorable characteristics. These materials are frequently activated through the addition of small amounts (e.g., a few hundred ppm) of elements such as thallium - or sodium in the case of CsI. The monovalent alkali halide scintillators can also be activated with low concentrations of Eu 2+, however Eu activation has previously not been widely employed due to the non-uniform segregation of the divalentmore » Eu dopant that leads to the formation of unwanted phases during Bridgman or other solidification crystal-growth methods. Specifically, for Eu concentrations near and above ~0.5%, Suzuki Phase precipitates form in the course of the melt-growth process, and these Suzuki Phase particles scatter the scintillation light. This adversely affects the scintillator performance via reduction in the optical transmission of the material, and depending on the crystal thickness and precipitated-particle concentration, this reduction can occur up to the point of opacity. Here we describe a post-growth process for the removal of Suzuki Phase precipitates from single crystals of the neutron scintillator LiI activated with Eu 2+ at concentrations up to and in excess of 3 wt.%, and we correlate the resulting neutron-detection performance with the thermal processing methods used to remove the Suzuki Phase particles. Furthermore, the resulting improved scintillator properties using increased Eu activator levels are applicable to neutron imaging and active interrogation systems, and pulse-height gamma-ray spectroscopy rather than pulse-shape discrimination can be used to discriminate between gamma ray and neutron interaction events.« less

Improved lithium iodide neutron scintillator with Eu2+ activation: The elimination of Suzuki-Phase precipitates

NASA Astrophysics Data System (ADS)

Boatner, L. A.; Comer, E. P.; Wright, G. W.; Ramey, J. O.; Riedel, R. A.; Jellison, G. E.; Kolopus, J. A.

2017-05-01

Monovalent alkali halides such as NaI, CsI, and LiI are widely used as inorganic scintillators for radiation detection due to their light yield, the capability for the growth of large single crystals, relatively low cost, and other favorable characteristics. These materials are frequently activated through the addition of small amounts (e.g., a few hundred ppm) of elements such as thallium - or sodium in the case of CsI. The monovalent alkali halide scintillators can also be activated with low concentrations of Eu2+, however Eu activation has previously not been widely employed due to the non-uniform segregation of the divalent Eu dopant that leads to the formation of unwanted phases during Bridgman or other solidification crystal-growth methods. Specifically, for Eu concentrations near and above 0.5%, Suzuki Phase precipitates form in the course of the melt-growth process, and these Suzuki Phase particles scatter the scintillation light. This adversely affects the scintillator performance via reduction in the optical transmission of the material, and depending on the crystal thickness and precipitated-particle concentration, this reduction can occur up to the point of opacity. Here we describe a post-growth process for the removal of Suzuki Phase precipitates from single crystals of the neutron scintillator LiI activated with Eu2+ at concentrations up to and in excess of 3 wt%, and we correlate the resulting neutron-detection performance with the thermal processing methods used to remove the Suzuki Phase particles. The resulting improved scintillator properties using increased Eu activator levels are applicable to neutron imaging and active interrogation systems, and pulse-height gamma-ray spectroscopy rather than pulse-shape discrimination can be used to discriminate between gamma ray and neutron interaction events.

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

Boatner, Lynn A.; Comer, Eleanor P.; Wright, Gomez W.

Monovalent alkali halides such as NaI, CsI, and LiI are widely used as inorganic scintillators for radiation detection due to their light yield, the capability for the growth of large single crystals, relatively low cost, and other favorable characteristics. These materials are frequently activated through the addition of small amounts (e.g., a few hundred ppm) of elements such as thallium - or sodium in the case of CsI. The monovalent alkali halide scintillators can also be activated with low concentrations of Eu 2+, however Eu activation has previously not been widely employed due to the non-uniform segregation of the divalentmore » Eu dopant that leads to the formation of unwanted phases during Bridgman or other solidification crystal-growth methods. Specifically, for Eu concentrations near and above ~0.5%, Suzuki Phase precipitates form in the course of the melt-growth process, and these Suzuki Phase particles scatter the scintillation light. This adversely affects the scintillator performance via reduction in the optical transmission of the material, and depending on the crystal thickness and precipitated-particle concentration, this reduction can occur up to the point of opacity. Here we describe a post-growth process for the removal of Suzuki Phase precipitates from single crystals of the neutron scintillator LiI activated with Eu 2+ at concentrations up to and in excess of 3 wt.%, and we correlate the resulting neutron-detection performance with the thermal processing methods used to remove the Suzuki Phase particles. Furthermore, the resulting improved scintillator properties using increased Eu activator levels are applicable to neutron imaging and active interrogation systems, and pulse-height gamma-ray spectroscopy rather than pulse-shape discrimination can be used to discriminate between gamma ray and neutron interaction events.« less

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

NASA Astrophysics Data System (ADS)

Vijayakumar, P.; Ramasamy, P.

2016-08-01

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

Exploration of New Principles in Spintronics Based on Topological Insulators (Option 1)

DTIC Science & Technology

2012-05-14

on the surface and found that our crystals are exceedingly homogeneous (Supplementary Information). The persistently narrow X - ray diffraction peaks...modified Bridgman method (see Supplementary Information for details). X - ray diffraction measurements indicated the monotonic shrinkage of a and c axis...and annealing at that temperature for 4 days. X - ray diffraction analyses confirmed that all the samples have the same crystal structure (R 3m

PbF2-based single crystals and phase diagrams of PbF2-MF2 systems (M = Mg, Ca, Sr, Ba, Cd)

NASA Astrophysics Data System (ADS)

Buchinskaya, I. I.; Fedorov, Pavel P.; Sobolev, B. P.

1997-07-01

Optical grade single crystals of Pb0.67Cd0.33F2 and Pb1-xCaxF2 (x less than 0.05) were grown by the Bridgman technique in graphite crucibles under fluorinating atmosphere of teflon pyrolysis products. For determinations of concentration areas of solid solutions, suitable for crystal growth, the phase interactions in the systems PbF2 with fluorides of alkaline-earth elements and Cd were studied by DTA and x-ray powder diffraction techniques. Phase diagrams were described by corresponding thermodynamic models. Transition from pure PbF2 to two- component Pb0.67Cd0.33F2 crystal is accompanied by some increase in radiation hardness of the latter and positive changes of mechanical characteristics (the Pb0.67Cd0.33F2 composition microhardness is 147 plus or minus 5 kg/mm2 that is 5 times that of a pure lead fluoride, 28 plus or minus 4 kg/mm2). These solid solutions have a cubic Fm3m fluorite-type lattice as a high-temperature modification of PbF2.

Effect of accelerated crucible rotation on the segregation of impurities in vertical Bridgman growth of multi-crystalline silicon

NASA Astrophysics Data System (ADS)

Bellmann, M. P.; Meese, E. A.; Arnberg, L.

2011-03-01

We have performed axisymmetric, transient simulations of the vertical Bridgman growth of mc-silicon to study the effect of the accelerated crucible rotation technique (ACRT) on the melt flow and impurity segregation. A solute transport model has been applied to predict the final segregation pattern of impurities in a circular ingot. The sinusoidal ACRT rotation cycle considered here suppresses mixing in the melt near the center, resulting in diffusion-limited mass transport. Therefore the radial impurity segregation is increased towards the center. The effect of increased radial segregation is intensified for low values of the Ekman time scale.

High compositional homogeneity of CdTe{sub x}Se{sub 1−x} crystals grown by the Bridgman method

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-01

We obtained high-quality CdTe{sub x}Se{sub 1−x} (CdTeSe) crystals from ingots grown by the vertical Bridgman technique. The compositional uniformity of the ingots was evaluated by X-ray fluorescence at BNL’s National Synchrotron Light Source X27A beam line. The compositional homogeneity was highly uniform throughout the ingot, and the effective segregation coefficient of Se was ∼1.0. This high uniformity offers potential opportunity to enhance the yield of the materials for both infrared substrate and radiation-detector applications, so greatly lowering the cost of production and also offering us the prospect to grow large-diameter ingots for use as large-area substrates and for producing highermore » efficiency gamma-ray detectors. The concentration of secondary phases was found to be much lower, by eight- to ten fold compared to that of conventional Cd{sub x}Zn{sub 1−x}Te (CdZnTe or CZT)« less

High Compositional Homogeneity of CdTe xSe 1-x Crystals Grown by the Bridgman Method

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-03

We obtained high-quality CdTe xSe 1-x (CdTeSe) crystals from ingots grown by the vertical Bridgman technique. The compositional uniformity of the ingots was evaluated by X-ray fluorescence at BNL’s National Synchrotron Light Source X27A beam line. The resulting compositional homogeneity was highly uniform throughout the ingot, and the effective segregation coefficient of Se was ~1.0. This uniformity offers potential opportunity to enhance the yield of the materials for both infrared substrate and radiation-detector applications, so greatly lowering the cost of production and also offering us the prospect to grow large-diameter ingots for use as large-area substrates and for producing highermore » efficiency gamma-ray detectors. The concentration of secondary phases was found to be much lower, by eight- to ten fold compared to that of conventional Cd xZn 1-xTe (CdZnTe or CZT).« less

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

NASA Astrophysics Data System (ADS)

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

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

Investigation on synthesis, growth, structure and physical properties of AgGa0.5In0.5S2 single crystals for Mid-IR application

NASA Astrophysics Data System (ADS)

Karunagaran, N.; Ramasamy, P.

2018-02-01

Silver Gallium Indium Sulfide (AgGa0.5In0.5S2) belongs to the family of AIBIIIC2VI ternary compound semiconductors which crystallize in the chalcopyrite structure. Synthesis of the polycrystalline material from the starting elements is achieved using melt temperature oscillation method. The AgGa0.5In0.5S2 single crystals have been grown by the vertical Bridgman technique. The synthesized AgGa0.5In0.5S2 polycrystalline charge was confirmed by powder XRD. The peak positions are in good agreement with the powder diffraction file. Thermal property was analyzed using differential scanning calorimetry (DSC) technique. The melting point of the crystal is 896 °C and freezing point is 862 °C. The unit cell parameters were confirmed by single crystal X-ray. The transmittance of the grown crystal is 55% in the NIR region and 60% in the mid-IR region. The optical band gap was found to be 2.0 eV. The stoichiometric composition of AgGa0.5In0.5S2 was measured using energy dispersive spectrometry (EDS). The photoluminescence behavior of AgGa0.5In0.5S2 has been analyzed. The resistivity of the grown single crystal has been measured.

New Scintillator Materials (K2CeBr5) and (Cs2CeBr5)

NASA Technical Reports Server (NTRS)

Hawrami, R.; Volz, M. P.; Batra, A. K.; Aggarwal, M. D.; Roy, U. N.; Groza, M.; Burger, A.; Cherepy, Nerine; Niedermayr, Thomas; Payne, Stephen A.

2008-01-01

Cesium cerium bromide (Cs2CeBr5) and potassium cerium bromide (K2CeBr5) are new scintillator materials for X-ray and gamma ray detector applications. Recently halide scintillator materials, such as Ce doped lanthanum bromide has been proved to be very important material for the same purpose. These materials are highly hygroscopic; a search for high light yield non-hygroscopic materials was highly desirable to advance the scintillator technology. In this paper, we are reporting the crystal growth of novel scintillator materials, cesium cerium bromide (Cs2CeBr5) and potassium cerium bromide (K2CeBr5). Crystals were successfully grown from the melt using the vertical Bridgman-Stockbarger technique, in a comparison with the high performance LaBr3 or LaCl3 crystals, cerium based alkali halides crystals, (Cs2CeBr5) and (K2CeBr5) have similar scintillation properties, while being much less hygroscopic. Furthermore, cesium based compounds will not suffer from the self-activity present in potassium and lanthanum compounds. However the Cs2CeBr5 crystals did not grow properly probably due to non-congruent melting or to some phase transition during cooling. Keywords." Scintillator materials; Ce3+; Energy resolution; Light yield; K2CeBr5

Crystal growth and near infrared optical properties of Pr 3+ doped lead halide materials for resonantly pumped eye safe laser applications

NASA Astrophysics Data System (ADS)

Jones, Ivy Krystal

In this dissertation the material development and optical spectroscopy of Pr3+ activated low phonon energy halide crystals is presented for possible applications in resonantly pumped eye-safe solid-state laser gain media. In the last twenty years, the developments in fiber and diode lasers have enabled highly efficient resonant pumping of Pr3+ doped crystals for possible lasing in the 1.6--1.7 microm region. In this work, the results of the purification, crystal growth, and near-infrared (NIR) spectroscopic characterization of Pr3+ doped lead (II) chloride, PbCl2 and lead (II) bromide, PbBr2 are presented. The investigated PbCl2 and PbBr2 crystals are non-hygroscopic with maximum phonon energies between ~180--200 cm-1, which enable efficient emission in the NIR spectral region (~ 1.6 microm) from the 3F3/3F4 → 3H4 transition of Pr3+ ions. The commercial available starting materials were purchased as ultra dry, high purity (~ 99.999 %) beads and purified through a combination of zone-refinement and halogenation. The crystal growth of Pr3+ doped PbCl 2 and PbBr2 was performed via vertical Bridgman technique using a two-zone furnace. The resulting Pr3+ doped PbCl 2 and PbBr2 crystals exhibited characteristic IR absorption bands in the 1.5--1.7 microm region (3H4 → 3F3/3F4), which allow for resonant pumping using commercial diode lasers. A broad IR emission band centered at ~1.6 microm was observed under ~1445 nm diode laser excitation from both Pr3+ doped halides. This dissertation presents comparative spectroscopic results for Pr 3+:PbCl2 and Pr3+:PbBr2 including NIR absorption and emission studies, lifetime measurements, modelling of radiative and non-radiative decay rates, determination of transition cross-section, and the net effective gain cross sections.

Design and Growth of Novel Compounds for Radiation Sensors: Multinary Chalcogenides

NASA Technical Reports Server (NTRS)

Singh, N. B.; Su, Ching-Hua; Nagaradona, Teja; Arnold, Brad; Choa, Fow-Sen

2016-01-01

Increasing threats of radiological weapons have revitalized the researches for low cost large volume ?-ray and neutron ray sensors In the past few years we have designed and grown ternary and quaternary lead and thallium chalcogenides and lead selenoiodides for detectors to meet these challenges. These materials are congruent, can be tailored to enhance the parameters required for radiation sensors. In addition, this class of compounds can be grown by Bridgman method which promises for large volume productions. We have single crystals of several compounds from the melt including Tl3AsSe3, Tl3AsSe3-xSx, TlGaSe2, AgGaGe3Se8, AgxLi1-xAgGaGe3Se8 and PbTlI5-x Sex compounds. Experimental studies indicate that these have very low absorption coefficient, low defect density and can be fabricated in any shape and sizes. These crystals do not require post growth annealing and do not show any second phase precipitates when processed for electrode bonding and other fabrication steps. In this paper we report purification, growth and fabrication of large Tl3AsSe3 (TAS) crystals. We observed that TAS crystals grown by using further purification of as supplied high purity source materials followed by directionally solidified charge showed higher resistivity than previously reported values. TAS also showed constant value as the function of voltage. A low thermal gradient and high purity source material were used to reduce thermal stresses in large crystals. By improving the purification of the as supplied source materials very high quality thallium, selenium and arsenic was achieved for preparing stoichiometric Tl3AsSe3 compound. Low gradient (<20K/cm) and slow growth rate (1-2 cm/day) produced crystals with reduced stress. Crystals did not show any micro cracking during fabrication of crystals grown with high purity and at low thermal gradient. Since thallium is a major component and very sensitive to surface oxidation, removal of surface and bulk oxides is very important. Intentional increase in the growth rate from 1cm/day to higher speed (>5cm/day) showed very different morphologies on the surface of the crystals. Electrical resistivity was one order of magnitude higher than previously reported value and it was observed to be constant as the function of frequency.

Transition metal doping of GaSe implemented with low temperature liquid phase growth

NASA Astrophysics Data System (ADS)

Lei, Nuo; Sato, Youhei; Tanabe, Tadao; Maeda, Kensaku; Oyama, Yutaka

2017-02-01

Our group works on improving the conversion efficiencies of terahertz (THz) wave generation using GaSe crystals. The operating principle is based on difference frequency generation (DFG) which has the advantages such as high output power, a single tunable frequency, and room temperature operation. In this study, GaSe crystals were grown by the temperature difference method under controlled vapor pressure (TDM-CVP). It is a liquid phase growth method with temperature 300 °C lower than that of the Bridgman method. Using this method, the point defects concentration is decreased and the polytype can be controlled. The transition metal Ti was used to dope the GaSe in order to suppress free carrier absorption in the low frequency THz region. As a result, a deep acceptor level of 38 meV was confirmed as being formed in GaSe with 1.4 at% Ti doping. Compared with undoped GaSe, a decrease in carrier concentration ( 1014 cm-3) at room temperature was also confirmed. THz wave transmittance measurements reveal the tendency for the absorption coefficient to increase as the amount of dopant is increased. It is expected that there is an optimum amount of dopant.

Sn-doped Bi1.1Sb0.9Te2S: An ideal bulk topological insulator

NASA Astrophysics Data System (ADS)

Kushwaha, Sk; Pletikosic, I.; Liang, T.; Gyenis, A.; Lapidus, Sh; Tian, Y.; Zhao, H.; Burch, Ks; Lin, J.; Wang, W.; Ji, H.; Fedorov, Av; Yazdani, A.; Ong, Np; Valla, T.; Cava, Rj

In the recent decade the topological insulators have been of significant importance for the condensed matter community. However, so far no real materials could fulfill all the requirements. Here, we present the Bridgman growth of slightly Sn-doped Bi1.1Sb0.9Te2S (with bulk band gap of 350) single crystals and characterization by electronic transport, STM and ARPES. The results on the crystals exhibit an intrinsic semiconducting behavior with the Fermi level and Dirac energies lie in bulk gap and high quality 2D surface states are detangled from the bulk states, and it fulfils all the requirements to be an ideal topological insulator. ARO MURI W911NF-12-1-0461; ARO W911NF-12-1-0461; MRSEC NSF-DMR-1420541; LBNL & BNL DE-AC02-05CH11231 & DE-SC0012704; DOE Office of Science DE-AC02-06CH11357; NSF DMR-1410846.

Finite-difference fluid dynamics computer mathematical models for the design and interpretation of experiments for space flight. [atmospheric general circulation experiment, convection in a float zone, and the Bridgman-Stockbarger crystal growing system

NASA Technical Reports Server (NTRS)

Roberts, G. O.; Fowlis, W. W.; Miller, T. L.

1984-01-01

Numerical methods are used to design a spherical baroclinic flow model experiment of the large scale atmosphere flow for Spacelab. The dielectric simulation of radial gravity is only dominant in a low gravity environment. Computer codes are developed to study the processes at work in crystal growing systems which are also candidates for space flight. Crystalline materials rarely achieve their potential properties because of imperfections and component concentration variations. Thermosolutal convection in the liquid melt can be the cause of these imperfections. Such convection is suppressed in a low gravity environment. Two and three dimensional finite difference codes are being used for this work. Nonuniform meshes and implicit iterative methods are used. The iterative method for steady solutions is based on time stepping but has the options of different time steps for velocity and temperature and of a time step varying smoothly with position according to specified powers of the mesh spacings. This allows for more rapid convergence. The code being developed for the crystal growth studies allows for growth of the crystal as the solid-liquid interface. The moving interface is followed using finite differences; shape variations are permitted. For convenience in applying finite differences in the solid and liquid, a time dependent coordinate transformation is used to make this interface a coordinate surface.

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

Aliev, Ziya S., E-mail: ziyasaliev@gmail.com; Institute of Physics, ANAS, H.Javid ave. 131, AZ1143 Baku; Donostia International Physics Center

Single crystals of the ternary copper compounds CuTlS and CuTlSe have been successfully grown from stoichiometric melt by using vertical Bridgman-Stockbarger method. The crystal structure of the both compounds has been determined by powder and single crystal X-Ray diffraction. They crystallize in the PbFCl structure type with two formula units in the tetragonal system, space group P4/nmm, a=3.922(2); c=8.123(6); Z=2 and a=4.087(6); c=8.195(19) Å; Z=2, respectively. The band structure of the reported compounds has been analyzed by means of full-potential linearized augmented plane-wave (FLAPW) method based on the density functional theory (DFT). Both compounds have similar band structures and aremore » narrow-gap semiconductors with indirect band gap. The resistivity measurements agree with a semiconductor behavior although anomalies are observed at low temperature. - Graphical abstract: The crystal structures of CuTl and CuTlSe are isostructural with the PbFCl-type and the superconductor LiFeAs-type tetragonal structure. The band structure calculations confirmed that they are narrow-gap semiconductors with indirect band gaps of 0.326 and 0.083 eV. The resistivity measurements, although confirming the semiconducting behavior of both compounds exhibit unusual anomalies at low temperatures. - Highlights: • Single crystals of CuTlS and CuTlSe have been successfully grown by Bridgman-Stockbarger method. • The crystal structure of the both compounds has been determined by single crystal XRD. • The band structure of the both compounds has been analyzed based on the density functional theory (DFT). • The resistivity measurements have been carried out from room temperature down to 10 K.« less

The Effect of the Traveling Magnetic Field (TMF) on the Buoyancy-Induced Convection in the Vertical Bridgman growth of Germanium

NASA Technical Reports Server (NTRS)

Yesilyurt, S.; Motakef, S.; Grugel, R.; Mazuruk, K.

2003-01-01

A traveling magnetic field (TMF) is created by means of applying out-of-phase currents to a number of coils. When applied to a conducting melt inside a cylindrical container, the TMF induces a Lorentz force that acts in the meridional directions (radial and axial), unlike the application of a rotating magnetic field (RMF), which creates a force in the azimuthal direction. In this work, we present a computational study of the TMF and its application to the Bridgman growth of the Ge. To quantify the effect of the TMF on the solid-melt interface, we use the maximum (magnitude-wise) tangential shear at the interface.

Numerical modeling of Bridgman growth of PbSnTe in a magnetic field

NASA Technical Reports Server (NTRS)

Yao, Minwu; Chait, Arnon; Fripp, Archibald L.; Debnam, William J.

1995-01-01

In this work we study heat and mass transport, fluid motion, and solid/liquid phase change in the process of steady Bridgman growth of Pb(.8)Sn(.2)Te (LTT) in an axially-imposed uniform magnetic field under terrestrial and microgravity conditions. In particular, this research is concerned with the interrelationships among segregation, buoyancy-driven convection, and magnetic damping in the LTT melt. The main objectives are to provide a quantitative understanding of the complex transport phenomena during solidification of the nondilute binary of LTT, to provide estimates of the strength of magnetic field required to achieve the desired diffusion-dominated growth, and to assess the role of magnetic damping for space and earth based control of the buoyancy-induced convection. The problem was solved by using FIDAP and numerical results for both vertical and horizontal growth configurations with respect to the acceleration of gravity vector are presented.

Thermoluminescence kinetic features of Lithium Iodide (LiI) single crystal grown by vertical Bridgman technique

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Kim, H. J.; Kim, Sunghwan; Khan, Sajid

2017-08-01

Single crystal of pure Lithium Iodide (LiI) has been grown from melt by using the vertical Bridgman technique. Thermoluminescence (TL) Measurements were carried out at 1 K/s following X-ray irradiation. The TL glow curve consists of a dominant peak at (peak-maximum Tm) 393 K and one low temperature peak of weaker intensity at 343 K. The order of kinetics (b), activation energy (E), and the frequency factor (S) for a prominent TL glow peak observed around 393 K for LiI crystals are reported for the first time. The peak shape analysis of the glow peak indicates the kinetics to be of the first order. The value of E is calculated using various standard methods such as initial rise (IR), whole glow peak (WGP), peak shape (PS), computerized glow curve deconvolution (CGCD) and Variable Heating rate (VHR) methods. An average value of 1.06 eV is obtained in this case. In order to validate the obtained parameters, numerically integrated TL glow curve has been generated using experimentally determined kinetic parameters. The effective atomic number (Zeff) for this material was determined and found to be 52. X-ray induced emission spectra of pure LiI single crystal are studied at room temperature and it is found that the sample exhibit sharp emission at 457 nm and broad emission at 650 nm.

Crystal growth and analysis of ohmic contact and magneto-optical isolator properties of cadmium manganese telluride

NASA Astrophysics Data System (ADS)

Prakasam, Mythili; Viraphong, Oudomsack; Teulé-Gay, Lionel; Decourt, Rodolphe; Veber, Philippe; Víllora, Encarnación G.; Shimamura, Kiyoshi

2011-03-01

Cd1-xMnxTe (x=0.1, 0.3, 0.5, 0.7 and 0.9) (CMT) single crystals were grown by the vertical Bridgman method. The optical studies reveal that with the increase in Mn concentration, the band gap values increase, which is attributed to s, p-d exchange interaction between the band carriers and Mn ions. Faraday rotation angle of the grown CMT (x=0.5) crystals were measured at the following wavelengths: 825, 1060 and 1575 nm. It was inferred that CMT exhibit larger Faraday effect (3-6 times larger than terbium-gallium garnet (TGG) currently used for optical isolators) making it as an efficient material for optical isolator at longer wavelengths. Field-cooled and zero field-cooled magnetizations of CMT were measured as a function of temperature and magnetic field. The spin-glass like behavior of CMT and their tendency to decrease in magnitude with increasing Mn concentration have been analyzed. The metal contacts on the Cd1-xMnxTe (x=0.1, 0.5, 0.7 and 0.9) crystals have been made with various metals and metal alloys to establish the ohmic contact. The detector characteristics of CMT have been tested using γ-rays with 511 keV (22 Na) and 59.5 keV (241 Am).

Crystal growth and dislocation etch pits observation of chalcopyrite CdSiP2

NASA Astrophysics Data System (ADS)

He, Zhiyu; Zhao, Beijun; Zhu, Shifu; Chen, Baojun; Huang, Wei; Lin, Li; Feng, Bo

2018-01-01

CdSiP2 is the only crystal that can offer Non-critical Phase Matching (NCPM) for a 1064 nm pumped optical parametric oscillation (OPO) with idler output in the 6 μm range. In this paper, a large, crack-free CdSiP2 single crystal measuring 18 mm in diameter and 65 mm in length was successfully grown by the Vertical Bridgman method (MVB) with an explosion-proof quartz ampoule. The results of lattice parameters, element composition and IR transmittance of the as-grown crystal characterized by X-ray diffraction (XRD), energy dispersive X-ray spectrometer (EDS) and Fourier transformation infrared spectrometer (FTIR) showed the as grown crystal crystallized well and the absorption coefficients at 4878 cm-1 and 2500 cm-1 were 0.14 cm-1 and 0.06 cm-1. Moreover, a new etchant composed of Br2, HCl, HNO3, CH3OH and H2O (1:800:800:400:400 in volume ratio) was prepared and the dislocation etch pits on oriented faces of as-grown CdSiP2 crystal were observed for the first time. It is found the etch pits are in rectangular structure on the (1 0 1) face, but in trigonal pyramid structure on (3 1 2) face. According to the quantities of the etch pits, the average densities of dislocation were evaluated to be 2.28 × 105/cm2 and 1.4 × 105/cm2, respectively.

Determination of the Contact Angle Based on the Casimir Effect

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Volz, Martin P.

2015-01-01

On a macroscopic scale, a nonreactive liquid partially covering a homogeneous solid surface will intersect the solid at an angle called the contact angle. For molten metals and semiconductors, the contact angle is materially dependent upon both the solid and liquid and typical values fall in the range 80-170 deg, depending on the crucible material. On a microscopic scale, there does not exist a precise and sharp contact angle but rather the liquid and solid surfaces merge smoothly and continuously. Consider the example of the so called detached Bridgman crystal growth process. In this technique, a small gap is formed between the growing crystal and the crucible. At the crystal/melt interface, a meniscus ring is formed. Its width can be in the range of a few micrometers, approaching a microscopic scale. It then becomes questionable to describe the shape of this meniscus by the contact angle. A more advanced treatment of the interface is needed and here we propose such a refined model. The interaction of the liquid surface with the solid can be calculated by considering two forces: a short-range repulsive force and a longer range (up to a few micrometers) Casimir or van der Waals force.

Comparison of the properties of tonpilz transducers fabricated with 001 fiber-textured lead magnesium niobate-lead titanate ceramic and single crystals.

PubMed

Brosnan, Kristen H; Messing, Gary L; Markley, Douglas C; Meyer, Richard J

2009-11-01

Tonpilz transducers are fabricated from 001 fiber-textured 0.72Pb(Mg(1/3)Nb(2/3))O(3)-0.28PbTiO(3) (PMN-28PT) ceramics, obtained by the templated grain growth process, and PMN-28PT ceramic and Bridgman grown single crystals of the same composition. In-water characterization of single element transducers shows higher source levels, higher in-water coupling, and more usable bandwidth for the 81 vol % textured PMN-28PT device than for the ceramic PMN-28PT element. The 81 vol % textured PMN-28PT tonpilz element measured under large signals shows linearity in sound pressure levels up to 0.23 MV/m drive field but undergoes a phase transition due to a lowered transition temperature from the SrTiO(3) template particles. Although the textured ceramic performs well in this application, it could be further improved with compositional tailoring to raise the transition temperature and better processing to improve the texture quality. With these improvements textured piezoelectric ceramics will be viable options for medical ultrasound, actuators, and sonar applications because of their ease of processing, compositional homogeneity, and potentially lower cost than single crystal.

Dendritic Growth Morphologies in Al-Zn Alloys—Part I: X-ray Tomographic Microscopy

NASA Astrophysics Data System (ADS)

Friedli, Jonathan; Fife, J. L.; di Napoli, P.; Rappaz, M.

2013-12-01

Upon solidification, most metallic alloys form dendritic structures that grow along directions corresponding to low index crystal axes, e.g., directions in fcc aluminum. However, recent findings[1,2] have shown that an increase in the zinc content in Al-Zn alloys continuously changes the dendrite growth direction from to in {100} planes. At intermediate compositions, between 25 wt pct and 55 wt pct Zn, dendrites and textured seaweeds were reported. The reason for this dendrite orientation transition is that this system exhibits a large solubility of zinc, a hexagonal metal, in the primary fcc aluminum phase, thus modifying its weak solid-liquid interfacial energy anisotropy. Owing to the complexity of the phenomenology, there is still no satisfactory theory that predicts all the observed microstructures. The current study is thus aimed at better understanding the formation of these structures. This is provided by the access to their 3D morphologies via synchrotron-based X-ray tomographic microscopy of quenched Bridgman solidified specimens in combination with the determination of the crystal orientation of the dendrites by electron-backscattered diffraction. Most interestingly, all alloys with intermediate compositions were shown to grow as seaweeds, constrained to grow mostly in a (001) symmetry plane, by an alternating growth direction mechanism. Thus, these structures are far from random and are considered less hierarchically ordered than common dendrites.

Crystal growth and electronic structure of low-temperature phase SrMgF{sub 4}

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

Atuchin, Victor V.; Functional Electronics Laboratory, Tomsk State University, Tomsk 634050; Laboratory of Semiconductor and Dielectric Materials, Novosibirsk State University, Novosibirsk 630090

2016-04-15

Using the vertical Bridgman method, the single crystal of low temperature phase SrMgF{sub 4} is obtained. The crystal is in a very good optical quality with the size of 10×7×5 mm{sup 3}. Detailed photoemission spectra of the element core levels are determined by a monochromatic AlKa (1486.6 eV) X-ray source. Moreover, the first-principles calculations are performed to investigate the electronic structure of SrMgF{sub 4}. A good agreement between experimental and calculated results is achieved. It is demonstrated that almost all the electronic orbitals are strongly localized and the hybridization with the others is very small, but the Mg–F bonds covalencymore » is relatively stronger than that of Sr–F bonds. - Graphical abstract: Large size of low-temperature phase SrMgF{sub 4} crystal was obtained (right) and its electronic structure was investigated by X-ray photoelectron spectroscopy and first-principles calculation (left). - Highlights: • Large size single crystal of low-temperature phase SrMgF{sub 4} is obtained. • Electronic structure of SrMgF{sub 4} is measured by X-ray photoelectron spectroscopy. • Partial densities of states are determined by first-principles calculation. • Good agreement between experimental and calculated results is achieved. • Strong ionic characteristics of chemical bonds are exhibited in SrMgF{sub 4}.« less

Crystal growth and furnace analysis

NASA Technical Reports Server (NTRS)

Dakhoul, Youssef M.

1986-01-01

A thermal analysis of Hg/Cd/Te solidification in a Bridgman cell is made using Continuum's VAST code. The energy equation is solved in an axisymmetric, quasi-steady domain for both the molten and solid alloy regions. Alloy composition is calculated by a simplified one-dimensional model to estimate its effect on melt thermal conductivity and, consequently, on the temperature field within the cell. Solidification is assumed to occur at a fixed temperature of 979 K. Simplified boundary conditions are included to model both the radiant and conductive heat exchange between the furnace walls and the alloy. Calculations are performed to show how the steady-state isotherms are affected by: the hot and cold furnace temperatures, boundary condition parameters, and the growth rate which affects the calculated alloy's composition. The Advanced Automatic Directional Solidification Furnace (AADSF), developed by NASA, is also thermally analyzed using the CINDA code. The objective is to determine the performance and the overall power requirements for different furnace designs.

The thermoelectric properties of bulk crystalline n- and p-type Mg2Si prepared by the vertical Bridgman method

NASA Astrophysics Data System (ADS)

Akasaka, Masayasu; Iida, Tsutomu; Matsumoto, Atsunobu; Yamanaka, Kohei; Takanashi, Yoshifumi; Imai, Tomohiro; Hamada, Noriaki

2008-07-01

Bulk Mg2Si crystals were grown using the vertical Bridgman melt growth method. The n-type and p-type dopants, bismuth (Bi) and silver (Ag), respectively, were incorporated during the growth. X-ray powder diffraction analysis revealed clear peaks of Mg2Si with no peaks associated with the metallic Mg and Si phases. Residual impurities and process induced contaminants were investigated by using glow discharge mass spectrometry (GDMS). A comparison between the results of GDMS and Hall effect measurements indicated that electrical activation of the Bi doping in the Mg2Si was sufficient, while activation of the Ag doping was relatively smaller. It was shown that an undoped n-type specimen contained a certain amount of aluminum (Al), which was due either to residual impurities in the Mg source or the incorporation of process-induced impurities. Thermoelectric properties such as the Seebeck coefficient and the electrical and thermal conductivities were measured as a function of temperature up to 850 K. The dimensionless figures of merit for Bi-doped and Ag-doped samples were 0.65 at 840 K and 0.1 at 566 K, respectively. Temperature dependence of the observed Seebeck coefficient was fitted well by the two-carrier model. The first-principles calculations were carried out by using the all-electron band-structure calculation package (ABCAP) in which the full-potential linearized augmented-plane-wave method was employed. The ABCAP calculation adequately presents characteristics of the Seebeck coefficients for the undoped and heavily Bi-doped samples over the whole measured temperature range from room temperature to 850 K. The agreement between the theory and the experiment is poorer for the Ag-doped p-type samples.

Analytical estimates of radial segregation in Bridgman growth from low-level steady and periodic accelerations

NASA Astrophysics Data System (ADS)

Naumann, Robert J.; Baugher, Charles

1992-08-01

Estimates of the convective flows driven by horizontal temperature gradients in the vertical Bridgman configuration are made for dilute systems subject to the low level accelerations typical of the residual accelerations experienced by a spacecraft in low Earth orbit. The estimates are made by solving the Navier-Stokes momentum equation in one dimension. The mass transport equation is then solved in two dimensions using a first-order perturbation method. This approach is valid provided the convective velocities are small compared to the growth velocity which generally requires a reduced gravity environment. If this condition is satisfied, there will be no circulating cells, and hence no convective transport along the vertical axis. However, the variations in the vertical velocity with radius will give rise to radial segregation. The approximate analytical model developed here can predict the degree of radial segregation for a variety of material and processing parameters to an accuracy well within a factor of two as compared against numerical computations of the full set of Navier-Stokes equations for steady accelerations. It has the advantage of providing more insight into the complex interplay of the processing parameters and how they affect the solute distribution in the grown crystal. This could be extremely valuable in the design of low-gravity experiments in which the intent is to control radial segregation. Also, the analysis can be extended to consider transient and periodic accelerations, which is difficult and costly to do numerically. Surprisingly, it was found that the relative radial segregation falls as the inverse cube of the frequency for periodic accelerations whose periods are short compared with the characteristic diffusion time.

Investigation of Cd1-xMgxTe as possible materials for X and gamma ray detectors

NASA Astrophysics Data System (ADS)

Mycielski, Andrzej; Kochanowska, Dominika M.; Witkowska-Baran, Marta; Wardak, Aneta; Szot, Michał; Domagała, Jarosław; Witkowski, Bartłomiej S.; Jakieła, Rafał; Kowalczyk, Leszek; Witkowska, Barbara

2018-06-01

In recent years, a series of investigations has been devoted to a possibility of using crystals based on CdTe with addition of magnesium (Mg) for X and gamma radiation detectors. Since we have had wide technological possibilities of preparing crystals and investigating their properties, we performed crystallizations of the crystals mentioned above. Thereafter, we investigated selected properties of the obtained materials. The crystallization processes were performed by using the Low Pressure Bridgman (LPB) method. The elements used: Cd, Te, Mg were of the highest purity available at present. In order to obtain reliable conclusions the crystallization processes were carried out at identical technological conditions. The details of our technological method and the results of the investigation of physical properties of the samples are presented below.

Interplay between magnetism and superconductivity in iron-chalcogenide superconductors: crystal growth and characterizations

NASA Astrophysics Data System (ADS)

Wen, Jinsheng; Xu, Guangyong; Gu, Genda; Tranquada, J. M.; Birgeneau, R. J.

2011-12-01

In this review, we present a summary of results on single crystal growth of two types of iron-chalcogenide superconductors, Fe1+yTe1-xSex (11), and AxFe2-ySe2 (A = K, Rb, Cs, Tl, Tl/K, Tl/Rb), using Bridgman, zone-melting, vapor self-transport and flux techniques. The superconducting and magnetic properties (the latter gained mainly from neutron scattering measurements) of these materials are reviewed to demonstrate the connection between magnetism and superconductivity. It will be shown that for the 11 system, while static magnetic order around the reciprocal lattice position (0.5, 0) competes with superconductivity, spin excitations centered around (0.5, 0.5) are closely coupled to the materials' superconductivity; this is made evident by the strong correlation between the spectral weight around (0.5, 0.5) and the superconducting volume fraction. The observation of a spin resonance below the superconducting temperature, Tc, and the magnetic-field dependence of the resonance emphasize the close interplay between spin excitations and superconductivity, similar to cuprate superconductors. In AxFe2-ySe2, superconductivity with Tc ~ 30 K borders an antiferromagnetic insulating phase; this is closer to the behavior observed in the cuprates but differs from that in other iron-based superconductors.

Magnetic flow control in growth and casting of photovoltaic silicon: Numerical and experimental results

NASA Astrophysics Data System (ADS)

Poklad, A.; Pal, J.; Galindo, V.; Grants, I.; Heinze, V.; Meier, D.; Pätzold, O.; Stelter, M.; Gerbeth, G.

2017-07-01

A novel, vertical Bridgman-type technique for growing multi-crystalline silicon ingots in an induction furnace is described. In contrast to conventional growth, a modified setup with a cone-shaped crucible and susceptor is used. A detailed numerical simulation of the setup is presented. It includes a global thermal simulation of the furnace and a local simulation of the melt, which aims at the influence of the melt flow on the temperature and concentration fields. Furthermore, seeded growth of cone-shaped Si ingots using either a monocrystalline seed or a seed layer formed by pieces of poly-Si is demonstrated and compared to growth without seeds. The influences of the seed material on the grain structure and the dislocation density of the ingots are discussed. The second part addresses model experiments for the Czochralski technique using the room temperature liquid metal GaInSn. The studies were focused on the influence of a rotating and a horizontally static magnetic field on the melt flow and the related heat transport in crucibles being heated from bottom and/or side, and cooled by a crystal model covering about 1/3 of the upper melt surface.

Steady state modeling of large diameter crystal growth using baffles

NASA Technical Reports Server (NTRS)

Sahai, Vivek; Williamson, John; Overfelt, Tony

1991-01-01

Buoyancy driven flow in the crystal melt is one of the leading causes of segregation. Natural convection arises from the presence of thermal and/or solutal gradients in the melt and it is not possible to completely eliminate the convection even in the low gravity environment of space. This paper reports the results of computational modeling research that is being done in preparation for space-based experiments. The commercial finite element code FIDAP was used to simulate the steady convection of a gallium-doped germanium alloy in a Bridgman-Stockbarger furnace. In particular, the study examines the convection-suppressing benefits of inserting cylindrical baffles in the molten region to act as viscous dampers. These thin baffles are assumed to be inert and noncontaminating. The results from this study show the manner in which the streamlines, velocities, and temperature fields at various gravity levels are affected by the presence of baffles. The effects of changing both the number and position of the baffles are examined and the advantages and disadvantages of using baffles are considered.

Directional Solidification of Mercury Cadmium Telluride During the Second United States Microgravity Payload Mission (USMP-2)

NASA Technical Reports Server (NTRS)

Gillies, D. C.; Lehoczky, S. L.; Szofran, F. R.; Watring, D. A.; Alexander, H. A.; Jerman, G. A.

1996-01-01

As a solid solution semiconductor having, a large separation between liquidus and solidus, mercury cadmium telluride (MCT) presents a formidable challenge to crystal growers desiring an alloy of high compositional uniformity. To avoid constitutional supercooling during Bridgman crystal growth it is necessary to solidify slowly in a high temperature gradient region. The necessary translation rate of less than 1 mm/hr results in a situation where fluid flow induced by gravity on earth is a significant factor in material transport. The Advanced Automated Directional Solidification Furnace (AADSF) is equipped to provide the stable thermal environment with a high gradient, and the required slow translation rate needed. Ground based experiments in AADSF show clearly the dominance of flow driven transport. The first flight of AADSF in low gravity on USMP-2 provided an opportunity to test theories of fluid flow in MCT and showed several solidification regimes which are very different from those observed on earth. Residual acceleration vectors in the orbiter during the mission were measured by the Orbital Acceleration Research Experiment (OARE), and correlated well with observed compositional differences in the samples.

Homogeneity of CdZnTe detectors

NASA Astrophysics Data System (ADS)

Hermon, H.; Schieber, M.; James, R. B.; Lund, J.; Antolak, A. J.; Morse, D. H.; Kolesnikov, N. N. P.; Ivanov, Y. N.; Goorsky, M. S.; Yoon, H.; Toney, J.; Schlesinger, T. E.

1998-02-01

We describe the current state of nuclear radiation detectors produced from single crystals of Cd 1- xZn xTe(CZT), with 0.04 < x < 0.4, grown by the vertical high pressure Bridgman (VHPB) method. The crystals investigated were grown commercially both in the USA and at the Institute of Solid State Physics, Chernogolska, Russia. The CZT was evaluated by Sandia National Laboratories and the UCLA and CMU groups using proton-induced X-ray emission (PIXE), X-ray diffraction (XRD), photoluminescence (PL), infrared (IR) transmission microscopy, leakage current measurements and response to nuclear radiation. We discuss the homogeneity of the various CZT crystals based on the results from these measurement techniques.

High-Performance Doped Strontium Iodide Crystal Growth Using a Modified Bridgman Method

NASA Astrophysics Data System (ADS)

Rowe, Emmanuel

The importance of gamma-ray spectroscopy---the science of determining the distribution of energy in a gamma field---can rarely be overstated. High performance scintillators for gamma-ray spectroscopy in Nuclear Nonproliferation applications and homeland security require excellent energy resolution to distinguish neighboring element and isotope lines while minimizing the time and exposure to do so. Semiconductor detectors operate by converting incident photons directly into electrical pulses, but often have problems of high costs due to constituent segregation and surface states as is the case for Cadmium Zinc Telluride. The ideal scintillator material for gamma spectrometer will therefore requires high light yield, excellent proportionality between light yield and gamma photon energy, and material uniformity. A scintillator should possess the following properties; it should convert the kinetic energy of the generated charged particles (typically K-shell electrons) into detectable visible light. This conversion should be linear-the light yield should be proportional to deposited energy over as wide a range as possible. For good light collection, the medium should be transparent to the wavelength of its own emission. The decay time of the induced luminescence should be short so that fast signal pulses can be generated. The medium should be of good optical quality and subject to manufacture in sizes large enough to be of interest as a practical detector. Its index of refraction should be near that of glass (~1.5) to permit efficient coupling of scintillation light to a photomultiplier tube or other photo-sensor. In the past decade, inorganic scintillator research has focused less on improving the characteristics of known scintillators, but rather on the search for new hosts capable of fast response and high energy resolution. Extensive searches have been made for hosts doped with lanthanide activators utilizing the allowed 5d-4f transition. These 5d-4f transitions are dipole-allowed and thus are about 106 times stronger than the more frequently observed 4f-4f transition in the trivalent rare earth ions. Ce3+, Nd3+ and Pr3+ have been investigated for fast response applications while Ce3+, Eu 2+, and Yb2+ stand out as the most promising activators offering high light yield, and high energy resolution. Using a modified Bridgman growth technique we have grown crystals with a low energy resolution of 2.6% at 662 keV, which is lower than the previous 2.8% reported for SrI2:Eu 2+. The modified technique (called so for its vertical crystal growth orientation) is necessary due to the anisotropic thermal expansion coefficient of Strontium Iodide. The problem plaguing the growth of the crystal is spontaneous cracking, which usually appear during cooling in the bulk. With the use of a zone separating shield, one can achieve more control of the temperature gradient between the two zones without compromising the actual temperature of the two zones. Additionally the use of codopants, in particular divalent magnesium improved the crystalline quality by acting as a gathering for iodine ions, which led to reduction of defect density.

Hierarchical microstructures in CZT

NASA Astrophysics Data System (ADS)

Sundaram, S. K.; Henager, C. H.; Edwards, D. J.; Schemer-Kohrn, A. L.; Bliss, M.; Riley, B. R.; Toloczko, M. B.; Lynn, K. G.

2011-10-01

Advanced characterization tools, such as electron backscatter diffraction and transmitted IR microscopy, are being applied to study critical microstructural features and orientation relations in as-grown CZT crystals to aid in understanding the relation between structure and properties in radiation detectors. Even carefully prepared single crystals of CZT contain regions of slight misorientation, Te-particles, and dislocation networks that must be understood for more accurate models of detector response. This paper describes initial research at PNNL into the hierarchy of microstructures observed in CZT grown via the vertical gradient freeze or vertical Bridgman method at PNNL and WSU.

Numerical modeling of melt flows in vertical Bridgman configuration affected by a rotating heat field

NASA Astrophysics Data System (ADS)

Kokh, K. A.; Popov, V. N.; Kokh, A. E.; Krasin, B. A.; Nepomnyaschikh, A. I.

2007-05-01

In this work, the numerical modeling of convection in a vertical Bridgman system under the influence of a rotating heat field was studied. First results show that changing of the heating from an axi-symmetric to a non-symmetric non-stationary configuration results in an increase in the convective flow and thus led to an increase of the melt uniformity because the convective cell is occupying almost the entire melt domain. Experimental growth of polycrystalline silicon under such special conditions provided ingots with improved texture and uniformity of electronic properties.

New high performing scintillators: RbSr2Br5:Eu and RbSr2I5:Eu

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Johnson, J.; Koschan, M.; Lukosi, E.; Melcher, C. L.

2017-11-01

We report the crystal growth and scintillation properties of two new ternary metal halide scintillators, RbSr2Br5 and RbSr2I5, activated with divalent europium. Transparent 7 mm diameter single crystals with 2.5% Eu2+ were grown in evacuated quartz ampoules via the Bridgman technique. RbSr2Br5 and RbSr2I5 have monoclinic crystal structures with densities of 4.18 g/cm3 and 4.55 g/cm3 respectively. These materials are hygroscopic and have some intrinsic radioactivity due to the presence of 87Rb. Luminescence properties typical of the 5d-4f radiative transition in Eu2+ were observed. The X-ray excited emissions consisted of singular peaks centered at 429 nm for RbSr2Br5:Eu 2.5% and 445 nm for RbSr2I4:Eu 2.5%. RbSr2Br5:Eu 2.5% had a light yield of 64,700 photons/MeV, with an energy resolution of 4.0%, and RbSr2I5:Eu 2.5% had a light yield of 90,400 ph/MeV with an energy resolution of 3.0% at 662 keV. Both crystals have an excellent proportional response over a wide range of gamma-ray energies.

Splitting Fermi Surfaces and Heavy Electronic States in Non-Centrosymmetric U3Ni3Sn4

NASA Astrophysics Data System (ADS)

Maurya, Arvind; Harima, Hisatomo; Nakamura, Ai; Shimizu, Yusei; Homma, Yoshiya; Li, DeXin; Honda, Fuminori; Sato, Yoshiki J.; Aoki, Dai

2018-04-01

We report the single-crystal growth of the non-centrosymmetric paramagnet U3Ni3Sn4 by the Bridgman method and the Fermi surface properties detected by de Haas-van Alphen (dHvA) experiments. We have also investigated single-crystal U3Ni3Sn4 by single-crystal X-ray diffraction, magnetization, electrical resistivity, and heat capacity measurements. The angular dependence of the dHvA frequencies reveals many closed Fermi surfaces, which are nearly spherical in topology. The experimental results are in good agreement with local density approximation (LDA) band structure calculations based on the 5f-itinerant model. The band structure calculation predicts many Fermi surfaces, mostly with spherical shape, derived from 12 bands crossing the Fermi energy. To our knowledge, the splitting of Fermi surfaces due to the non-centrosymmetric crystal in 5f-electron systems is experimentally detected for the first time. The temperature dependence of the dHvA amplitude reveals a large cyclotron effective mass of up to 35 m0, indicating the heavy electronic state of U3Ni3Sn4 due to the proximity of the quantum critical point. From the field dependence of the dHvA amplitude, a mean free path of conduction electrons of up to 1950 Å is detected, reflecting the good quality of the grown crystal. The small splitting energy related to the antisymmetric spin-orbit interaction is most likely due to the large cyclotron effective mass.

Axisymmetry breaking instabilities of natural convection in a vertical bridgman growth configuration

NASA Astrophysics Data System (ADS)

Gelfgat, A. Yu.; Bar-Yoseph, P. Z.; Solan, A.

2000-12-01

A study of the three-dimensional axisymmetry-breaking instability of an axisymmetric convective flow associated with crystal growth from bulk of melt is presented. Convection in a vertical cylinder with a parabolic temperature profile on the sidewall is considered as a representative model. The main objective is the calculation of critical parameters corresponding to a transition from the steady axisymmetric to the three-dimensional non-axisymmetric (steady or oscillatory) flow pattern. A parametric study of the dependence of the critical Grashof number Gr cr on the Prandtl number 0⩽Pr⩽0.05 (characteristic for semiconductor melts) and the aspect ratio of the cylinder 1⩽ A⩽4 ( A=height/radius) is carried out. The stability diagram Grcr(Pr, A) corresponding to the axisymmetric — three-dimensional transition is reported for the first time. The calculations are done using the spectral Galerkin method allowing an effective and accurate three-dimensional stability analysis. It is shown that the axisymmetric flow in relatively low cylinders tends to be oscillatory unstable, while in tall cylinders the instability sets in due to a steady bifurcation caused by the Rayleigh-Benard mechanism. The calculated neutral curves are non-monotonous and contain hysteresis loops. The strong dependence of the critical Grashof number and the azimuthal periodicity of the resulting three-dimensional flow indicate the importance of a comprehensive parametric stability analysis in different crystal growth configurations. In particular, it is shown that the first instability of the flow considered is always three-dimensional.

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

NASA Technical Reports Server (NTRS)

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

2002-01-01

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2 at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS). The purpose of the microgravity experiments includes differentiating among proposed mechanisms contributing to detachment, and confirming or refining our understanding of the detachment mechanism. Because large contact angle are critical to detachment, sessile drop measurements were used to determine the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases from 150 deg to an equilibrium value of 117 deg (Ge) or from 129 deg to an equilibrium value of 100 deg (GeSi) over the duration of the experiment. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. Results in this presentation will show that we have established the effects on detachment of ampoule material, pressure difference above and below the melt, and silicon concentration; samples that are nearly completely detached can be grown repeatedly in pBN.

Effect of steady crucible rotation on the segregation of impurities in vertical Bridgman growth of multi-crystalline silicon

NASA Astrophysics Data System (ADS)

Bellmann, M. P.; Meese, E. A.

2011-10-01

We have performed axisymmetric, transient simulations of the vertical Bridgman growth of multi-crystalline (mc) silicon to study the effect of the steady crucible rotation on the melt flow and impurity segregation. A solute transport model has been applied to predict the final segregation pattern of impurities in a circular ingot. Imposing rotation rates of 1-5 rpm on the system makes radial segregation much worse compared to the non-rotating case. Low rotation rates at 1-2 rpm increase radial segregation in the first half period of solidification, whereas at rotation rates above the effect is insignificantly small. Contrary behavior was observed for the second half period of solidification. Here radial segregation is increased at high rotation rates from 3 to 5 rpm with small impact at 1-2 rpm.

Finite Element Analysis of Magnetic Damping Effects on G-Jitter Induced Fluid Flow

NASA Technical Reports Server (NTRS)

Pan, Bo; Li, Ben Q.; deGroh, Henry C., III

1997-01-01

This paper reports some interim results on numerical modeling and analyses of magnetic damping of g-jitter driven fluid flow in microgravity. A finite element model is developed to represent the fluid flow, thermal and solute transport phenomena in a 2-D cavity under g-jitter conditions with and without an applied magnetic field. The numerical model is checked by comparing with analytical solutions obtained for a simple parallel plate channel flow driven by g-jitter in a transverse magnetic field. The model is then applied to study the effect of steady state g-jitter induced oscillation and on the solute redistribution in the liquid that bears direct relevance to the Bridgman-Stockbarger single crystal growth processes. A selection of computed results is presented and the results indicate that an applied magnetic field can effectively damp the velocity caused by g-jitter and help to reduce the time variation of solute redistribution.

Reducing and Inducing Convection in Ge-Si Melts with Static Magnetic Field

NASA Technical Reports Server (NTRS)

Szofran, Frank R.

1999-01-01

Results of a study of the effectiveness of using static magnetic fields to reduce convection in Ge-Si melts will be presented. Lenz's law causes a retardation of convection when a static magnetic field is applied to an electrically conducting liquid. However, during the solidification of a solid-solution system such as Ge-Si, the interface is neither isothermal nor isoconcentrational. The variation of temperature and chemical composition along the interface causes thermoelectric currents to be generated within the solidifying material (and the container if it is electrically conductive). These currents, in the presence of a magnetic field, can cause movement (stirring, convection) in the melt which can exceed convection induced by normal thermosolutal mechanisms. Crystals have been grown by both the Bridgman and floating-zone methods. Clear evidence for the existence of this thermoelectromagnetic convection, especially in the case of Si floating-zone growth, will be presented.

Numerical analysis of impurity separation from waste salt by investigating the change of concentration at the interface during zone refining process

NASA Astrophysics Data System (ADS)

Choi, Ho-Gil; Shim, Moonsoo; Lee, Jong-Hyeon; Yi, Kyung-Woo

2017-09-01

The waste salt treatment process is required for the reuse of purified salts, and for the disposal of the fission products contained in waste salt during pyroprocessing. As an alternative to existing fission product separation methods, the horizontal zone refining process is used in this study for the purification of waste salt. In order to evaluate the purification ability of the process, three-dimensional simulation is conducted, considering heat transfer, melt flow, and mass transfer. Impurity distributions and decontamination factors are calculated as a function of the heater traverse rate, by applying a subroutine and the equilibrium segregation coefficient derived from the effective segregation coefficients. For multipass cases, 1d solutions and the effective segregation coefficient obtained from three-dimensional simulation are used. In the present study, the topic is not dealing with crystal growth, but the numerical technique used is nearly the same since the zone refining technique was just introduced in the treatment of waste salt from nuclear power industry because of its merit of simplicity and refining ability. So this study can show a new application of single crystal growth techniques to other fields, by taking advantage of the zone refining multipass possibility. The final goal is to achieve the same high degree of decontamination in the waste salt as in zone freezing (or reverse Bridgman) method.

Magnetic Field Suppression of Flow in Semiconductor Melt

NASA Technical Reports Server (NTRS)

Fedoseyev, A. I.; Kansa, E. J.; Marin, C.; Volz, M. P.; Ostrogorsky, A. G.

2000-01-01

One of the most promising approaches for the reduction of convection during the crystal growth of conductive melts (semiconductor crystals) is the application of magnetic fields. Current technology allows the experimentation with very intense static fields (up to 80 KGauss) for which nearly convection free results are expected from simple scaling analysis in stabilized systems (vertical Bridgman method with axial magnetic field). However, controversial experimental results were obtained. The computational methods are, therefore, a fundamental tool in the understanding of the phenomena accounting during the solidification of semiconductor materials. Moreover, effects like the bending of the isomagnetic lines, different aspect ratios and misalignments between the direction of the gravity and magnetic field vectors can not be analyzed with analytical methods. The earliest numerical results showed controversial conclusions and are not able to explain the experimental results. Although the generated flows are extremely low, the computational task is a complicated because of the thin boundary layers. That is one of the reasons for the discrepancy in the results that numerical studies reported. Modeling of these magnetically damped crystal growth experiments requires advanced numerical methods. We used, for comparison, three different approaches to obtain the solution of the problem of thermal convection flows: (1) Spectral method in spectral superelement implementation, (2) Finite element method with regularization for boundary layers, (3) Multiquadric method, a novel method with global radial basis functions, that is proven to have exponential convergence. The results obtained by these three methods are presented for a wide region of Rayleigh and Hartman numbers. Comparison and discussion of accuracy, efficiency, reliability and agreement with experimental results will be presented as well.

Thermoelectric Behavior of PbSe Single Crystals

DOE PAGES

Kogo, Gilbert; Pradhan, Aswini K.; Roy, Utpal N.

2016-12-05

The electrical conductivity and Seebeck coefficient of PbSe single crystals grown by the Bridgman technique display metallic behavior. The Seebeck coefficient increases linearly with increasing temperature and showed positive Seebeck values, typically valid for a p-type PbSe crystal. The electronic thermal conductivity decreases with increase in temperature. The power factor increases gradually with temperature until the maximum value of 6.51 × 10 -3 W/mK2 at 260 K, other values are 5.95 × 10 -3 W/mK 2 at 300 K, and 5.40 × 10 -3 W/mK 2 at 320 K. Our results demonstrate that as-grown PbSe crystal is generically p-type duemore » to excess in Pb and can be a potential candidate for thermoelectric power generation.« less

Effect of axial magnetic field on three-dimensional instability of natural convection in a vertical Bridgman growth configuration

NASA Astrophysics Data System (ADS)

Gelfgat, A. Yu.; Bar-Yoseph, P. Z.; Solan, A.

2001-08-01

A study of the effect of an externally imposed magnetic field on the axisymmetry-breaking instability of an axisymmetric convective flow, associated with crystal growth from bulk of melt, is presented. Convection in a vertical cylinder with a parabolic temperature profile on the sidewall is considered as a representative model. A parametric study of the dependence of the critical Grashof number Gr cr on the Hartmann number Ha for fixed values of the Prandtl number (Pr=0.015) and the aspect ratio of the cylinder ( A=height/radius=1, 2 and 3) is carried out. The stability diagram Gr cr(Ha) corresponding to the axisymmetric—three-dimensional transition for increasing values of the axial magnetic field is obtained. The calculations are done using the spectral Galerkin method allowing an effective and accurate three-dimensional stability analysis. It is shown that at relatively small values of Ha the axisymmetric flow tends to be oscillatory unstable. After the magnitude of the magnetic field (Ha) exceeds a certain value the instability switches to a steady bifurcation caused by the Rayleigh-Bénard mechanism.

Magnetically Orchestrated Formation of Diamond at Lower Temperatures and Pressures

NASA Astrophysics Data System (ADS)

Little, Reginald B.; Lochner, Eric; Goddard, Robert

2005-01-01

Man's curiosity and fascination with diamonds date back to ancient times. The knowledge of the many properties of diamond is recorded during Biblical times. Antoine Lavoisier determined the composition of diamond by burning in O2 to form CO2. With the then existing awareness of graphite as carbon, the race began to convert graphite to diamond. The selective chemical synthesis of diamond has been pursued by Cagniard, Hannay, Moisson and Parson. On the basis of the thermodynamically predicted equilibrium line of diamond and graphite, P W Bridgman attempted extraordinary conditions of high temperature (>2200°C) and pressure (>100,000 atm) for the allotropic conversion of graphite to diamond. H T Hall was the first to successfully form bulk diamond by realizing the kinetic restrictions to Bridgman's (thermodynamic) high pressure high temperature direct allotropic conversion. Moreover, Hall identified catalysts for the faster kinetics of diamond formation. H M Strong determined the import of the liquid catalyst during Hall's catalytic synthesis. W G Eversole discovered the slow metastable low pressure diamond formation by pyrolytic chemical vapor deposition with the molecular hydrogen etching of the rapidly forming stable graphitic carbon. J C Angus determined the import of atomic hydrogen for faster etching for faster diamond growth at low pressure. S Matsumoto has developed plasma and hot filament technology for faster hydrogen and carbon radical generations at low pressure for faster diamond formation. However the metastable low pressure chemical vapor depositions by plasma and hot filament are prone to polycrystalline films. From Bridgman to Hall to Eversole, Angus and Matsumoto, much knowledge has developed of the importance of pressure, temperature, transition metal catalyst, liquid state of metal (metal radicals atoms) and the carbon radical intermediates for diamond synthesis. Here we advance this understanding of diamond formation by demonstrating the external magnetic organization of carbon, metal and hydrogen radicals for lower temperature and pressure synthesis. Here we show that strong static external magnetic field (>15 T) enhances the formation of single crystal diamond at lower pressure and even atmospheric pressure with implications for much better, faster high quality diamond formation by magnetization of current high pressure and temperature technology.

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Schweizer, M.; Kaiser, N.; Cobb, S. D.; Motakef, S.; Vujisic, L. J.; Croell, A.; Dold, P.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS) to differentiate among proposed mechanisms contributing to detachment. Sessile drop measurements were first carried out for a large number of substrates made of potential ampoule materials to determine the contact angles and the surface tension as a function of temperature and composition. The process atmosphere and duration of the experiment (for some cases) were also found to have significant influence on the wetting angle. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases to an equilibrium value with duration of measurement ranging from 150 to 117 deg (Ge), 129 to 100 deg (GeSi). Forming gas (Ar + 2% H2) and vacuum have been used in the growth ampoules. With gas in the ampoule, a variation of the temperature profile during growth has been used to control the pressure difference between the top of the melt and the volume below the melt caused by detachment of the growing crystal. The stability of detachment has been modeled and substantial insight has been gained into the reasons that detachment has most often been observed in reduced gravity but nonetheless has occurred randomly even there. An empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed and will be presented. Methods for determining the nature and extent of detachment include profilometry and optical and electron microscopy. This surface study is the subject of another presentation at this Congress. Results in this presentation will show that we have established the effects of different ampoule materials, temperature profiles, pressure differences, and silicon concentrations and that samples that are nearly completely detached can be grown repeatedly.

Scintillation properties of Eu 2+-doped KBa 2I 5 and K 2BaI 4

DOE PAGES

Stand, L.; Zhuravleva, M.; Chakoumakos, Bryan C.; ...

2015-09-25

We report two new ternary metal halide scintillators, KBa 2I 5 and K 2BaI 4, activated with divalent europium. Single crystal X-ray diffraction measurements confirmed that KBa 2I 5 has a monoclinic structure (P2 1/c) and that K 2BaI 4 has a rhombohedral structure (R3c). Differential scanning calorimetry showed singular melting and crystallization points, making these compounds viable candidates for melt growth. We grew 13 mm diameter single crystals of KBa 2I 5:Eu 2+ and K 2BaI 4:Eu2+ in evacuated quartz ampoules via the vertical Bridgman technique. The optimal Eu 2+ concentration was 4% for KBa 2I 5 and 7%more » for K 2BaI 4. The X-ray excited emissions at 444 nm for KBa 2I 5:Eu 4% and 448 nm for K 2BaI 4:Eu 7% arise from the 5d-4f radiative transition in Eu 2+. KBa 2I 5:Eu 4% has a light yield of 90,000 photons/MeV, with an energy resolution of 2.4% and K 2BaI 4:Eu 7% has a light yield of 63,000 ph/MeV, with an energy resolution of 2.9% at 662 keV. Both crystals have an excellent proportional response to a wide range of gamma-ray energies.« less

Effect of a Nonplanar Melt-Solid Interface On Lateral Compositional Distribution During Unidirectional Solidification of a Binary Alloy with a Constant Growth Velocity V. Pt. 1; Theory

NASA Technical Reports Server (NTRS)

Wang, Jai-Ching; Watring, D.; Lehoczky. S. L.; Su, C. H.; Gillies, D.; Szofran, F.; Sha, Y. G.; Sha, Y. G.

1999-01-01

Infrared detected materials, such as Hg(1-x)Cd(x)Te, Hg(1-x)Zn(x)Te have energy gaps almost linearly proportional to their composition. Due to the wide separation of liquidus and solidus curves of their phase diagram, there are compositional segregation in both of the axial and radial directions of these crystals grown in the Bridgman system unidirectionally with constant growth rate. It is important to understand the mechanisms, which affect lateral segregation such that large radially uniform composition crystal can be produced. Following Coriel, etc's treatment, we have developed a theory to study the effect of a curved melt-solid interface shape on lateral composition distribution. The model is considered to be a cylindrical system with azimuthal symmetry and a curved melt-solid interface shape which can be expressed as a linear combination of a series of Bessell's functions. The results show that melt-solid interface shape has a dominant effect on the lateral composition distribution of these systems. For small values of beta, the solute concentration at the melt-solid interface scales linearly with interface shape with a proportional constant of the produce of beta and (1 -k), where beta = VR/D, with V as growth velocity, R as the sample radius, D as the diffusion constant and k as the distribution constant. A detailed theory will be presented. A computer code has been developed and simulations have been performed and compared with experimental results. These will be published in another paper.

Effect of a Nonplanar Melt-Solid Interface on Lateral Compositional Distribution during Unidirectional Solidification of a Binary Alloy with a Constant Growth Velocity V. Part 1; Theory

NASA Technical Reports Server (NTRS)

Wang, Jai-Ching; Watring, Dale A.; Lehoczky, Sandor L.; Su, Ching-Hua; Gillies, Don; Szofran, Frank

1999-01-01

Infrared detector materials, such as Hg(1-x)Cd(x)Te, Hg(1-x)Zn(x)Te have energy gaps almost linearly proportional to its composition. Due to the wide separation of liquidus and solidus curves of their phase diagram, there are compositional segregations in both of axial and radial directions of these crystals grown in the Bridgman system unidirectionally with constant growth rate. It is important to understand the mechanisms which affect lateral segregation such that large uniform radial composition crystal is possible. Following Coriell, etc's treatment, we have developed a theory to study the effect of a curved melt-solid interface shape on the lateral composition distribution. The system is considered to be cylindrical system with azimuthal symmetric with a curved melt-solid interface shape which can be expressed as a linear combination of a series of Bessell's functions. The results show that melt-solid interface shape has a dominate effect on lateral composition distribution of these systems. For small values of b, the solute concentration at the melt-solid interface scales linearly with interface shape with a proportional constant of the product of b and (1 - k), where b = VR/D, with V as growth velocity, R as sample radius, D as diffusion constant and k as distribution constant. A detailed theory will be presented. A computer code has been developed and simulations have been performed and compared with experimental results. These will be published in another paper.

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

DOE PAGES

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

1996-08-01

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

Ellipsometry study of optical parameters of AgIn5S8 crystals

NASA Astrophysics Data System (ADS)

Isik, Mehmet; Gasanly, Nizami

2015-12-01

AgIn5S8 crystals grown by Bridgman method were characterized for optical properties by ellipsometry measurements. Spectral dependence of optical parameters; real and imaginary parts of the pseudodielectric function, pseudorefractive index, pseudoextinction coefficient, reflectivity and absorption coefficient were obtained from ellipsometry experiments carried out in the 1.2-6.2 eV range. Direct band gap energy of 1.84 eV was found from the analysis of absorption coefficient vs. photon energy. The oscillator energy, dispersion energy and zero-frequency refractive index, high-frequency dielectric constant values were found from the analysis of the experimental data using Wemple-DiDomenico and Spitzer-Fan models. Crystal structure and atomic composition ratio of the constituent elements in the AgIn5S8 crystal were revealed from structural characterization techniques of X-ray diffraction and energy dispersive spectroscopy.

Investigation of emission properties of doped aromatic derivative organic semiconductor crystals

NASA Astrophysics Data System (ADS)

Stanculescu, A.; Mihut, L.; Stanculescu, F.; Alexandru, H.

2008-04-01

Fluorescence measurements have been made on pure and doped bulk, mechanically polished wafers of crystalline m-DNB and benzil obtained by cutting ingots grown by the Bridgman-Stockbarger method modified for organic compounds crystallization. By comparison with pure matrices, we have investigated the effect of an inorganic dopant (iodine, silver, sodium) and of an organic dopant (m-DNB, naphthalene) on the emission characteristics (position and shape) of these molecular crystals. A slight shift of the emission peaks through high energy and an intense emission peak situated around 2.35 eV correlated with the local trapping level attributed to structural defects, which are involved in radiative processes, have been evidenced in iodine-doped m-DNB. The emission peak of m-DNB-doped benzil situated in the high-energy range (2.97 eV) is associated with direct emission activity of m-DNB, suggesting that this is an active impurity in benzil molecular matrix. We have not observed in benzil any evidence of indirect action of the impurity molecules (atoms) associated with the traps represented by the structural defects that generate changes in the energy levels of the neighbouring molecules and are correlated with different growth conditions. We have not remarked any involvement of the studied inorganic metallic impurities and of some organic impurities, such as naphthalene, in the radiative recombination processes in benzil matrix.

Identification of oxygen-related midgap level in GaAs

NASA Technical Reports Server (NTRS)

Lagowski, J.; Lin, D. G.; Gatos, H. C.; Aoyama, T.

1984-01-01

An oxygen-related deep level ELO was identified in GaAs employing Bridgman-grown crystals with controlled oxygen doping. The activation energy of ELO is almost the same as that of the dominant midgap level: EL2. This fact impedes the identification of ELO by standard deep level transient spectroscopy. However, it was found that the electron capture cross section of ELO is about four times greater than that of EL2. This characteristic served as the basis for the separation and quantitative investigation of ELO employing detailed capacitance transient measurements in conjunction with reference measurements on crystals grown without oxygen doping and containing only EL2.

Five Bit, Five Gigasample TED Analog-to-Digital Converter Development.

DTIC Science & Technology

1981-06-01

pliers. TRW uses two sources at present: materials grown by Horizontal I Bridgman technique from Crystal Specialties, and Czochralski from MRI. The...the circuit modelling and circuit design tasks. A number of design iterations were required to arrive at a satisfactory design. In or-der to riake...made by modeling the TELD as a voltage-controlled current generator with a built-in time delay between impressed voltage and output current. Based on

Time-of-Flight Measurements on TlBr Detectors

NASA Astrophysics Data System (ADS)

Suzuki, K.; Shorohov, M.; Sawada, T.; Seto, S.

2015-04-01

Carrier transport properties of TlBr crystals grown using the Bridgman method were investigated by the time-of-flight technique. The electron and hole mobilities were measured as 20 - 27 cm2 /Vs and 1.0 - 2.0 cm2/Vs respectively at room temperature. The temperature dependence of the electron mobility increases with decreasing temperature as approximated by a well-known empirical formula reflecting the reciprocal of the LO-phonon density.

Nonstoichiometry and luminescent properties of ZnSe crystals grown from the melt at high pressures

NASA Astrophysics Data System (ADS)

Khanh, Tran; Mozhevitina, Elena; Khomyakov, Andrew; Avetisov, Roman; Davydov, Albert; Chegnov, Vladimir; Antonov, Vladimir; Kobeleva, Svetlana; Zhavoronkov, Nikolai; Avetissov, Igor

2017-01-01

50 mm diameter ZnSe crystals have been grown from the melt by a vertical Bridgman technique at 100 atm argon pressure in a graphite crucible. 3D impurities concentration and nonstoichiometry mappings of the grown crystals have been defined by ICP-MS and a direct physic-chemical method, correspondingly. Photoluminescence mapping of the analyzed crystal has been done. It was found out that along the crystal height the nonstoichiometry changed from Se excess over stoichiometrical composition in the cone (bottom) part to Zn excess in the tail (upper) part passing through the stoichiometrical composition in the cylindrical part of the crystal. Metal impurities concentrated in the upper part of the crystal. The gas-forming impurities (H, C, O, N, F) had stochastic distribution but Cl impurity concentrated in the crystal peripheral part (near the crucible walls). It was found out that the as-grown crystal had a single wide PL peal with maximum of 583 nm. A proposal about complex structure luminescent center based on Cl dopant an overstoichiometric Se has been made.

Optical and transient capacitance study of EL2 in the absence and presence of other midgap levels. [in gallium arsenide crystals

NASA Technical Reports Server (NTRS)

Skowronski, M.; Lagowski, J.; Gatos, H. C.

1986-01-01

A high-resolution optical study was carried out on GaAs crystals grown by horizontal Bridgman and liquid-encapsulated-Czochralski methods. An excellent correlation was found between the intensity of the 1.039-eV no-phonon line and the characteristic absorption of EL2, the major deep donor level in GaAs. A correlation was also found between the characteristic optical absorption of EL2 and its concentration as determined by junction capacitance measurements. The presence of EL0, another midgap level contained in heavily oxygen-doped crystals at concentration always less than those of EL2, had no effect on the optical spectra, but altered the capacitance measurements. Accordingly, an accurate calibration for the determination of EL2 by optical absorption was obtained from capacitance measurements on crystals containing only EL2; in this way the uncertainties introduced by other midgap levels were eliminated.

Study of vibrational modes in CuxAg1-xIn5S8 mixed crystals by infrared reflection measurements

NASA Astrophysics Data System (ADS)

Gasanly, N. M.

2018-04-01

Infrared reflection spectra of CuxAg1-xIn5S8 mixed crystals, grown by Bridgman method, were studied in the wide frequency range of 50-2000 cm-1. All four infrared-active modes were detected, which are in full agreement with the prediction of group-theoretical analysis. Real and imaginary parts of the dielectric function, refractive index and the energy losses function were evaluated from reflectivity measurements. The frequencies of TO and LO modes and oscillator strengths were also determined. The bands detected in IR spectra of studied crystals were assigned to various vibration types (valence and valence-deformation) on the basis of the symmetrized displacements of atoms obtained employing the Melvin projection operators. The linear dependencies of optical mode frequencies on the composition of CuxAg1-xIn5S8 mixed crystals were obtained. These dependencies display one-mode behavior.

Cesium hafnium chloride: A high light yield, non-hygroscopic cubic crystal scintillator for gamma spectroscopy

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

Burger, Arnold, E-mail: aburger@fisk.edu; Department of Physics and Astronomy, Vanderbilt University, Nashville, Tennessee 37235; Rowe, Emmanuel

We report on the scintillation properties of Cs{sub 2}HfCl{sub 6} (cesium hafnium chloride or CHC) as an example of a little-known class of non-hygroscopic compounds having the generic cubic crystal structure of K{sub 2}PtCl{sub 6}. The crystals are easily growable from the melt using the Bridgman method with minimal precursor treatments or purification. CHC scintillation is centered at 400 nm, with a principal decay time of 4.37 μs and a light yield of up to 54 000 photons/MeV when measured using a silicon CCD photodetector. The light yield is the highest ever reported for an undoped crystal, and CHC also exhibits excellent lightmore » yield nonproportionality. These desirable properties allowed us to build and test CHC gamma-ray spectrometers providing energy resolution of 3.3% at 662 keV.« less

Microstructure and Mechanical Properties of Al2O3/Er3Al5O12 Binary Eutectic Ceramic Prepared by Bridgman Method

PubMed Central

Song, Caiyu; Wang, Shunheng; Liu, Juncheng; Zhai, Shuoyan

2018-01-01

Directionally solidified Al2O3/Er3Al5O12 (EAG) eutectic ceramic was prepared via vertical Bridgman method with high-frequency induction heating. The effects of the growth rate on the microstructure and mechanical properties of the solidified ceramic were investigated. The experimental results showed that there were no pores or amorphous phases in the directionally solidified Al2O3/EAG eutectic ceramic. Al2O3 phase was embedded in the EAG matrix phase, and the two phases were intertwined with each other to form a typical binary eutectic “hieroglyphic” structure. With the increase of growth rate, the phase size and spacing of the solidified Al2O3/EAG ceramic both decreased, and the growth rate and phase spacing satisfied the λ2v ≈ 60 formula of Jackson-Hunt theory. The cross section microstructure of the solidified ceramic always exhibited an irregular eutectic growth, while the longitudinal section microstructure presented a directional growth. The mechanical properties of the solidified ceramic gradually increased with the increase of growth rate, and the maximum hardness and fracture toughness could reach 21.57 GPa and 2.98 MPa·m1/2 respectively. It was considered that the crack deflection and branching could enhance the toughness of the solidified ceramic effectively. PMID:29601545

Analysis of low gravity tolerance of model experiments for space station: Preliminary results for directional solidification

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.; Ouazzani, Jalil

1988-01-01

It has become clear from measurements of the acceleration environment in the Spacelab that the residual gravity levels on board a spacecraft in low Earth orbit can be significant and should be of concern to experimenters who wish to take advantage of the low gravity conditions on future Spacelab missions and on board the Space Station. The basic goals are to better understand the low gravity tolerance of three classes of materials science experiments: crystal growth from a melt, a vapor, and a solution. The results of the research will provide guidance toward the determination of the sensitivity of the low gravity environment, the design of the laboratory facilites, and the timelining of materials science experiments. To data, analyses of the effects of microgravity environment were, with a few exceptions, restricted to order of magnitude estimates. Preliminary results obtained from numerical models of the effects of residual steady and time dependent acceleration are reported on: heat, mass, and momentum transport during the growth of a dilute alloy by the Bridgman-Stockbarger technique, and the response of a simple fluid physics experiment involving buoyant convection in a square cavity.

Optical and structural properties of indium doped bismuth selenide thin films

NASA Astrophysics Data System (ADS)

Pavagadhi, Himanshu; Vyas, S. M.; Patel, Piyush; Patel, Vimal; Patel, Jaydev; Jani, M. P.

2015-08-01

In: Bi2Se3 crystals were grown by Bridgman method at a growth velocity of 0.5cm/h with temperature gradient of 650 C/cm in our laboratory. The thin films of In:Bi2se3 were grown on amorphous substrate (glass) at a room temperature under a pressure of 10-4Pa by thermal evaporation technique. Thin film were deposited at various thicknesses and optical absorption spectrum of such thin films, obtain in wave no. range 300 to 2600 cm-1. The optical energy gap calculated from this data were found to be inverse function of square of thickness, particularly for thickness about 1800 Å or less. This dependence is explained in terms of quantum size effect. For thicker films, the bandgap is found to be independent of film thickness. For the surface stud of the as grown thin film by using AFM, which shows continuous film with some step height and surface roughness found in terms of few nm and particle size varies with respect to thickness.

Single crystal growth, electronic structure and optical properties of Cs2HgBr4

NASA Astrophysics Data System (ADS)

Lavrentyev, A. A.; Gabrelian, B. V.; Vu, V. T.; Shkumat, P. N.; Parasyuk, O. V.; Fedorchuk, A. O.; Khyzhun, O. Y.

2015-10-01

We report on successful synthesis of high-quality single crystal of cesium mercury tetrabromide, Cs2HgBr4, by using the vertical Bridgman-Stockbarger method as well as on studies of its electronic structure. For the Cs2HgBr4 crystal, we have recorded X-ray photoelectron spectra for both pristine and Ar+ ion-bombarded surfaces. Our data indicate that the Cs2HgBr4 single crystal surface is rather sensitive with respect to Ar+ ion-bombardment. In particular, such a treatment of the Cs2HgBr4 single crystal surface alters its elemental stoichiometry. To explore peculiarities of the energy distribution of total and partial densities of states within the valence band and the conduction band of Cs2HgBr4, we have made band-structure calculations based on density functional theory (DFT) employing the augmented plane wave+local orbitals (APW+lo) method as incorporated in the WIEN2k package. The APW+lo calculations allow for concluding that the Br 4p states make the major contributions in the upper portion of the valence band, while its lower portion is dominated by contributors of the Hg 5d and Cs 5p states. Further, the main contributors to the bottom of the conduction band of Cs2HgBr4 are the unoccupied Br p and Hg s states. In addition, main optical characteristics of Cs2HgBr4 such as dispersion of the absorption coefficient, real and imaginary parts of dielectric function, electron energy-loss spectrum, refractive index, extinction coefficient and optical reflectivity have been explored from the first-principles band-structure calculations.

1000 to 1200 K time-dependent compressive deformation of single-crystalline and polycrystalline B2 Ni-40Al

NASA Technical Reports Server (NTRS)

Whittenberger, J. D.; Noebe, R. D.; Kumar, K. S.; Mannan, S. K.; Cullers, C. L.

1991-01-01

The 1000-K and 1200-K time-dependent deformation of 100-line-oriented and non-100-line-oriented single crystals of Ni-40Al (made by a modified Bridgman technique) was examined over a large range of strain rates (from 0.1 to 10 to the -7th per sec). The results were compared with those for polycrystalline Ni-40Al made by hot pressing XD synthesized powder. The results from measurements of slow-plastic-strain-rate properties of the two materials show that single crystals offer no strength advantage over polycrystalline material. Both forms were found to deform via a dislocation climb mechanism.

Single-Crystal Bismuth Iodide Gamma-Ray Spectrometers

DTIC Science & Technology

2012-02-01

the density of the crystal (g/cm\\ M is the molecular weight of the vapor (g/mole), and R is the gas constant (cai/(K·mole)). Equation (6) indicates...along the vertical axis with a fixed rate. This simulated the downward movement of the ampoule in the conventional vertical Bridgman method. The...3cl512 1.03 4512 4.6 961 Pd Pd3d 336.5 Pd 3d512 1.03 6796 4.6 1477 Pdb N3d 340.3 Pd 3d3J2 1.03 2978 4.6 647 Pd Pd3d 341.7 Pd 3d3J2 1.03 4486 4.6 975

Magnetostriction and corrosion studies in single crystals of iron-gallium alloys

NASA Astrophysics Data System (ADS)

Jayaraman, Tanjore V.

Iron-gallium alloys have an excellent combination of large low-field magnetostriction, good mechanical properties, low hysteresis, and relatively low cost. This dissertation focuses on the magneto striction and corrosion behaviors of single crystals of Fe-Ga alloys. In the first part, the variation of magnetostrictive coefficient: (3/2) lambda100, with composition and heat treatment conditions of Fe-Ga alloys, is examined. Single crystals with compositions Fe-15 at.% Ga, Fe-20 at.% Ga, and Fe-27.5 at.% Ga were obtained by (a) vertical Bridgman technique (DG) and (b) vertical Bridgman technique followed by long-term annealing (LTA) and quenching. Rapid quenching from a phase region improves the (3/2) lambda 100 value in these alloys. X-ray diffraction characterization showed for the first time the direct evidence of short-range ordering in these alloys. The second part reports the first study of alpha" ordering heat treatment on the elastic properties and magnetostriction of Fe-27.5 at.% Ga alloy single crystals. The elastic constants were measured using resonant ultrasound spectroscopy (RUS), and the elastic properties and magneto-elastic coupling constant were calculated. The (3/2) lambda100 and B1 values obtained for a phase were higher than alpha" phase. The third part examines the first study of corrosion behavior of as-cast FeGa and Fe-Ga-Al alloys in acidic, basic, and simulated seawater environments. Corrosion measurements were performed by Tafel scan and polarization resistance method and in general exhibited good corrosion resistance. The fourth part examines the first study of corrosion behavior of Fe-15 at.% Ga, Fe-20 at.% Ga, and Fe-27.5 at.% Ga DG and LTA alloy single crystals and the dependence of corrosion rates on the crystal orientations. The corrosion resistance was better in basic environments followed by simulated seawater and acidic environments. The fifth part examines the effect of magnetostriction on the corrosion behavior of [100]-oriented single crystal of Fe-20 at.% Ga alloy in acidic and simulated seawater solution, first study ever of this kind. Magnetostrictive strain introduced on the application of saturation magnetic field increased the corrosion rate of [100]-oriented Fe-20 at.% Ga alloy single crystal by 40% in 0.1M HCl and decreased the corrosion rate by 15% in 3.5 wt.% NaCl solution.

Scintillation properties of a 2-inch diameter KCa0.8Sr0.2I3:Eu2+ single crystal

NASA Astrophysics Data System (ADS)

Wu, Yuntao; Lindsey, Adam C.; Loyd, Matthew; Stand, Luis; Zhuravleva, Mariya; Koschan, Merry; Melcher, Charles L.

2017-09-01

Inch-sized scintillating crystals are required for practical radiation detectors such as hand-held radio-isotope identification devices. In this work, a transparent and colorless 2-inch diameter KCa0.8Sr0.2I3: 0 . 5 mo% Eu2+ single crystal was grown by the vertical Bridgman method, and the scintillation properties of a ∅ 50 mm × 45 mm long sample were evaluated. The Eu2+ 5d1- 4 f emission under X-ray excitation is centered at 472 nm. Its scintillation decay time under 137 Cs source irradiation is 2 . 37 μs, and the absolute light output is 51,000 ± 3000 photons/MeV. The energy resolution at 662 keV was evaluated for different orientations of the crystals with respect to the PMT, and the effect of 40 K background subtraction on energy resolution was evaluated. The performance of the packaged crystal was also investigated.

Fermi surfaces of the pyrite-type cubic AuSb2 compared with split Fermi surfaces of the ullmannite-type cubic chiral NiSbS and PdBiSe

NASA Astrophysics Data System (ADS)

Nishimura, K.; Kakihana, M.; Nakamura, A.; Aoki, D.; Harima, H.; Hedo, M.; Nakama, T.; Ōnuki, Y.

2018-05-01

We grew high-quality single crystals of AuSb2 with the pyrite (FeS2)-type cubic structure by the Bridgman method and studied the Fermi surface properties by the de Haas-van Alphen (dHvA) experiment and the full potential LAPW band calculation. The Fermi surfaces of AuSb2 are found to be similar to those of NiSbS and PdBiSe with the ullmannite (NiSbS)-type cubic chiral structure because the crystal structures are similar each other and the number of valence electrons is the same between two different compounds. Note that each Fermi surface splits into two Fermi surfaces in NiSbS and PdBiSe, reflecting the non-centrosymmetric crystal structure.

Growth and magnetooptical properties of anisotropic TbF3 single crystals

NASA Astrophysics Data System (ADS)

Valiev, Uygun V.; Karimov, Denis N.; Burdick, Gary W.; Rakhimov, Rakhim; Pelenovich, Vasiliy O.; Fu, Dejun

2017-06-01

This paper investigates the Faraday effect and absorption and luminescence spectra of single-crystal TbF3 measured at 90 K and 300 K. The optical-quality single-phase TbF3 crystals (structural type β-YF3) were grown by the Bridgman technique. Faraday rotation angles were measured at remagnetization along the [100] crystallographic axis. Low temperature optical measurements were carried out along the [100] axis. "Quasi-doublet" sublevels with energy at 0 cm-1, 65 cm-1, and 190 cm-1, and also a singlet sublevel with energy at 114 cm-1 located in the ground 7F6 multiplet were determined from the low temperature luminescence spectra. The Van-Vleck behavior of the magnetic susceptibility χb can be satisfactorily explained by the magnetic mixing of wave functions belonging to the ground and first excited "quasi-doublet" sublevels at 0 and 65 cm-1, respectively. Analysis of the oscillation dependences of the rotation angle showed that the value of the natural birefringence (Δn ≈ 0.0186) remains nearly constant within the wavelength and temperature ranges under investigation. As the temperature decreases, we find significant increases in the oscillation amplitude of the rotation angle and in the Verdet constant V. The spectral dependences V(χ) are linear throughout the temperature range. The magnetooptical activity of TbF3 can be explained by means of the spin- and parity-allowed electric-dipole 4f → 5d transitions in the Tb3+ ions.

Characterization of Structural Defects in Wide Band-Gap Compound Materials for Semiconductor and Opto-Electronic Applications

NASA Astrophysics Data System (ADS)

Goue, Ouloide Yannick

Single crystals of binary and ternary compounds are touted to replace silicon for specialized applications in the semiconductor industry. However, the relative high density of structural defects in those crystals has hampered the performance of devices built on them. In order to enhance the performance of those devices, structurally perfect single crystals must be grown. The aim of this thesis is to investigate the interplay between crystal growth process and crystal quality as well as structural defect types and transport property. To this end, the thesis is divided into two parts. The first part provides a general review of the theory of crystal growth (chapter I), an introduction to the materials being investigated (chapter II and III) and the characterization techniques being used (chapter IV). • In chapter I, a brief description of the theory of crystal growth is provided with an eye towards the driving force behind crystal nucleation and growth along with the kinetic factors affecting crystal growth. The case of crystal growth of silicon carbide (SiC) by physical vapor transport (PVT) and chemical vapor deposition (CVD) is discussed. The Bridgman, travelling heater method (THM) and physical transport growth of cadmium zinc telluride (CZT) is also treated. In chapters II and III, we introduce the compound materials being investigated in this study. While a description of their crystal structure and properties is provided, the issues associated with their growth are discussed. In chapter IV, a description of the characterization techniques used in these studies is presented. These techniques are synchrotron X-ray topography (SXRT), transmission electron microscopy, transmission infrared microscopy (TIM), micro-Raman spectroscopy (muRS) and light microscopy. Extensive treatment of SXRT technique is also provided. In the second part, the experimental results obtained in the course of these studies are presented and discussed. These results are divided into three subsections. • The development of a new technique for the production of large and high quality silicon carbide single crystal boule is proposed. This technique herein referred to as Large Tapered Crystal (LTC) growth consists of two steps: growth of long SiC rod crystal by solvent-laser heated floating zone (Solvent-LHFZ) and lateral expansion of a seed by hot wall chemical vapor deposition (HWCVD). Solvent-LHFZ was successful as SiC rod crystals, replicating the polytype structure of the starting seed, were achieved at a growth rate varying from 4 to 100mum/hr. However, SXRT revealed the presence of an inhomogeneous strain in the grown crystal rod. This was further confirmed by SEM images, which showed the platelet-like morphology of the growth front with pockets in which iron (Fe)-rich material from the Fe solvent is trapped. It was furthermore observed that at high Fe to Si ratio (˜1.9), no growth was achieved. HWCVD enlargement was also successful as SiC boules, replicating the polytype structure of the starting seed, were achieved at growth rate of about 180mum/hr. The boules had a faceted hexagonal morphology with a strain-free surface marked by steps. Combination of SXRT, TEM and muRS revealed the presence of stacking disorder in the seed (3C, 4H and 15R-SiC) that replicated in the homoepitaxial layer. The formation of the observed stacking disorder is attributed to the low energy difference between stacking configurations on the growth surface as proposed by Takahashi and Ohtani. • The influence of structural defect type and distribution on minority carrier lifetime in 4H-SiC epilayers was investigated. Structural defect type and distribution map was obtained using SXRT, whereas minority carrier lifetime map was obtained using muPCD. Decrease in carrier lifetime observed from muPCD map was associated with specific structural defects such as low angle grain boundaries (LAGBs), stacking faults (SFs), interfacial dislocations (IDs), half loop arrays (HLAs) as well as basal plane dislocations (BPDs) pinned at TSDs. While the effect of morphological defects was mitigated, combination of defects such as microcracks, overlapping triangular defects and BPD half loops were observed to reduce carrier lifetime. Furthermore, regions of high dislocation density were associated with low carrier lifetime. • Finally, the effect of cadmium (Cd) overpressure on the quality of cadmium zinc telluride crystal ingots was investigated for two set of samples (set 1 and 2). Overall, high resistivity single crystals were achieved. Evaluation of the crystal quality by SXRT revealed that under certain Cd overpressures and growth conditions, the quality of the grown boule improved. Similarly, transmission infrared (IR) microscopy showed a correlation between the size/density and distribution of Te inclusions/precipitates and Cd overpressure. The size of Te inclusions was observed to decrease as a function of Cd overpressure as predicted from partial pressure data for stoichiometric melt. The best improvement in crystalline quality were observed for samples from set 1at a Cd reservoir of 785 °C and for set 2 samples for a Cd reservoir at 825 °C. This difference in Cd reservoir temperature for stoichiometric growth between set 1 and set 2 was attributed to other factors such as rate of cooling of Cd reservoir, rate of cooling of the crystal along with control of the melt interface. The summary of these results and the implication of this growth approach for producing high quality CZT single crystals are discussed.

Scintillation characterization of the pure Tl2LiGdBr6 single crystal

NASA Astrophysics Data System (ADS)

Jang, Jonghun; Rooh, Gul; Kim, Sunghwan; Kim, HongJoo

2018-05-01

A pure Tl2LiGdBr6 (TLGB) single crystal was developed. This scintillator was grown by the two-zone vertical Bridgman technique. Owing to the improvement in the crystal quality of TLGB, excellent scintillation properties were observed. The characterization of this scintillation material was carried out under X- and γ-ray excitations. In the X-ray excitation emission spectrum, the Tl+ ion emission band was observed between 390 and 550 nm and peaked at 435 nm. Under 662 keV γ-ray excitation, the energy resolution and light yield of the grown sample were measured to be 7.2% (FWHM) and 27,000 ± 2,700 ph/MeV, respectively. In addition, under the same γ-ray excitation, scintillation decay time was also measured at room temperature. Three decay time components were found to be 56 ns (24%), 105 ns (53%), and 1.5 µs (23%). Further improvements in scintillation properties are expected with the good quality crystal of this compound.

Comparative study of nondoped and Eu-doped SrI2 scintillator

NASA Astrophysics Data System (ADS)

Yanagida, Takayuki; Koshimizu, Masanori; Okada, Go; Kojima, Takahiro; Osada, Junya; Kawaguchi, Noriaki

2016-11-01

Optical and scintillation properties of nondoped and Eu 3% doped SrI2 crystals grown by the Vertical Bridgman method were investigated. Eu-doped crystal showed an intense single band emission at 430 nm due to the Eu2+ 5d-4f transitions in both photoluminescence and scintillation while the nondoped crystal had a complex spectral shape. The latter emission consists of mainly four bands: 360 nm, 540 nm, 410 nm and 430 nm. The origins of 360 nm and 540 nm were self-trapped exciton and unexpected impurity, respectively. The origins of 410 and 430 nm lines were ascribed to F center in different I sites. Under 137Cs γ-ray irradiations, both crystals showed a clear photoabsorption peak. The scintillation light yields of the nondoped and Eu-doped SrI2 resulted 33,000 ph/MeV and 82,000 ph/MeV, respectively. The energy resolution at 662 keV of Eu-doped was 4% while that of the non-doped SrI2 was 8%.

Mercury Chalcohalide Semiconductor Hg 3Se 2Br 2 for Hard Radiation Detection

DOE PAGES

Li, Hao; Meng, Fang; Malliakas, Christos D.; ...

2016-09-28

We present Hg 3Se 2Br 2 that has a wide band gap semiconductor (2.22 eV) with high density (7.598 g/cm 3) and crystallizes in the monoclinic space group C2/m with cell parameters of a = 17.496 (4) Å, b = 9.3991 (19) Å, c = 9.776(2) Å, β = 90.46(3)°, V = 1607.6(6) Å 3. It melts congruently at a low temperature, 566°C, which allows for an easy single crystal growth directly from the stoichiometric melt. Single crystals of Hg 3Se 2Br 2 up to 1 cm long have been grown using the Bridgman method. Hg 3Se 2Br 2 singlemore » crystals exhibit a strong photocurrent response when exposed to Ag X-ray and blue diode laser. The resistivity of Hg 3Se 2Br 2 measured by the two probe method is on the order of 10 11 Ω·cm, and the mobility-lifetime product (μτ) of the electron and hole carriers estimated from the energy spectroscopy under Ag X-ray radiation are (μτ) e ≈ 1.4 × 10 –4cm 2/V and (μτ) h ≈ 9.2 × 10 –5cm 2/V. Electronic structure calculations at the density functional theory level indicate a direct band gap and a relatively small effective mass for carriers. Lastly, on the basis of the photoconductivity and hard X-ray spectrum, Hg 3Se 2Br 2 is a promising candidate for X-ray and γ-ray radiation detection at room temperature.« less

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

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

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

DOE PAGES

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang; ...

2018-05-14

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Estimates of effects of residual acceleration on USML-1 experiments

NASA Technical Reports Server (NTRS)

Naumann, Robert J.

1995-01-01

The purpose of this study effort was to develop analytical models to describe the effects of residual accelerations on the experiments to be carried on the first U.S. Microgravity Lab mission (USML-1) and to test the accuracy of these models by comparing the pre-flight predicted effects with the post-flight measured effects. After surveying the experiments to be performed on USML-1, it became evident that the anticipated residual accelerations during the USML-1 mission were well below the threshold for most of the primary experiments and all of the secondary (Glovebox) experiments and that the only set of experiments that could provide quantifiable effects, and thus provide a definitive test of the analytical models, were the three melt growth experiments using the Bridgman-Stockbarger type Crystal Growth Furnace (CGF). This class of experiments is by far the most sensitive to low level quasi-steady accelerations that are unavoidable on space craft operating in low earth orbit. Because of this, they have been the drivers for the acceleration requirements imposed on the Space Station. Therefore, it is appropriate that the models on which these requirements are based are tested experimentally. Also, since solidification proceeds directionally over a long period of time, the solidified ingot provides a more or less continuous record of the effects from acceleration disturbances.

Resistivity dependence on Zn concentration in semi-insulating (Cd,Zn)Te

NASA Astrophysics Data System (ADS)

Fiederle, Michael; Fauler, Alex; Babentsov, Vladimir N.; Franc, Jan; Benz, Klaus Werner

2003-01-01

The resistivity dependence on Zn concentration had been investigated in semi-insulating (Cd,Zn)Te crystals grown by the vertical Bridgman method. A coorelation between the zinc concentration and the resistivity distribution could be found. The obtained resistivity was in the interval of 2 ×109-1010 Ω cm as expected from the model of compensation. The main deep compensating levels detected by Photo Induced Current Transient Spectroscopy (PICTS) were at 0.64 +/- 0.02 eV and close the middle of the band gap at 0.80 +/- 0.02 eV.

Magnetic Damping of Solid Solution Semiconductor Alloys

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Croell, Arne; Dold, Peter; Cobb, Sharon D.; Volz, Martin P.; Motakef, Shariar

1999-01-01

The objective of this study is to: (1) experimentally test the validity of the modeling predictions applicable to the magnetic damping of convective flows in electrically conductive melts as this applies to the bulk growth of solid solution semiconducting materials; and (2) assess the effectiveness of steady magnetic fields in reducing the fluid flows occurring in these materials during processing. To achieve the objectives of this investigation, we are carrying out a comprehensive program in the Bridgman and floating-zone configurations using the solid solution alloy system Ge-Si. This alloy system has been studied extensively in environments that have not simultaneously included both low gravity and an applied magnetic field. Also, all compositions have a high electrical conductivity, and the materials parameters permit reasonable growth rates. An important supporting investigation is determining the role, if any, that thermoelectromagnetic convection (TEMC) plays during growth of these materials in a magnetic field. TEMC has significant implications for the deployment of a Magnetic Damping Furnace in space. This effect will be especially important in solid solutions where the growth interface is, in general, neither isothermal nor isoconcentrational. It could be important in single melting point materials, also, if faceting takes place producing a non-isothermal interface. In conclusion, magnetic fields up to 5 Tesla are sufficient to eliminate time-dependent convection in silicon floating zones and possibly Bridgman growth of Ge-Si alloys. In both cases, steady convection appears to be more significant for mass transport than diffusion, even at 5 Tesla in the geometries used here. These results are corroborated in both growth configurations by calculations.

Process modelling for Space Station experiments

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.; Rosenberger, Franz; Nadarajah, Arunan; Ouazzani, Jalil; Amiroudine, Sakir

1990-01-01

Examined here is the sensitivity of a variety of space experiments to residual accelerations. In all the cases discussed the sensitivity is related to the dynamic response of a fluid. In some cases the sensitivity can be defined by the magnitude of the response of the velocity field. This response may involve motion of the fluid associated with internal density gradients, or the motion of a free liquid surface. For fluids with internal density gradients, the type of acceleration to which the experiment is sensitive will depend on whether buoyancy driven convection must be small in comparison to other types of fluid motion, or fluid motion must be suppressed or eliminated. In the latter case, the experiments are sensitive to steady and low frequency accelerations. For experiments such as the directional solidification of melts with two or more components, determination of the velocity response alone is insufficient to assess the sensitivity. The effect of the velocity on the composition and temperature field must be considered, particularly in the vicinity of the melt-crystal interface. As far as the response to transient disturbances is concerned, the sensitivity is determined by both the magnitude and frequency of the acceleration and the characteristic momentum and solute diffusion times. The microgravity environment, a numerical analysis of low gravity tolerance of the Bridgman-Stockbarger technique, and modeling crystal growth by physical vapor transport in closed ampoules are discussed.

MCT: A UK Retrospective—Reminiscences of a Crystal Grower

NASA Astrophysics Data System (ADS)

Capper, Peter

2017-09-01

The essentials of bulk Bridgman growth of mercury cadmium telluride (MCT) are outlined, together with some background to its use in the UK. It is still being used in a few niche applications, e.g., long-wavelength photoconductive (PC) detectors for space programs, and as material for infrared (IR) optical components. The latter requires very short-wavelength and/or larger-diameter material, and the challenges and successes in these areas are outlined. Use of a new source of high-purity silica, together with continual improvements in element purification, from our in-house tellurium zone refining and mercury distillation, reduced the carrier concentration consistently to sub-1014 cm-3, which helped to further improve PC device performance. An offer is made to supply bulk wafers to the wider community for research and development (R&D) purposes. The benefits of IR-related books, published over the past 30 years, to the community are described and a challenge laid down to continue this process of information dissemination into the future, in either hard-copy form or online versions.

Spectroscopic ellipsometric studies of the dielectric function of Cd1-x-yMnxFeyTe single crystals

NASA Astrophysics Data System (ADS)

Hwang, Younghun; Kim, Hyekyeong; Um, Youngho; Park, Hyoyeol

2004-06-01

Cd1-x-yMnxFeyTe single crystals grown by the vertical Bridgman method have been studied by measuring the complex dielectric function using spectroscopic ellipsometry in the 1.5 5.5 eV photon energy range at room temperature. The CP energy parameters of the E0, E1, E1 + 1, and E2 structures were determined by fitting the second-derivative spectra (d2/d2) with a theoretical model, i.e., the standard critical point (SCP) line shapes. The E1, E1 + 1, and E2 energies decreased with increasing Fe composition y, which is due to the hybridization effect of the valence and conduction bands in Cd1-xMnxTe with Fe 3d levels.

Intrinsic light yield and light loss coefficient of Bi4Ge3O12 single crystals

NASA Astrophysics Data System (ADS)

Yawai, Nattasuda; Chewpraditkul, Weerapong; Wanarak, Chalerm; Nikl, Martin; Ratanatongchai, Wichian

2014-10-01

In this paper we present the scintillation properties of polished Bi4Ge3O12 (BGO) crystals grown by the Bridgman method. The light yield (LY) and energy resolution were measured using XP5200B photomultiplier. At 662 keV γ-rays, high LY of 9680 photons/MeV and good energy resolution of 8.6% were obtained for a 5 × 5 × 1 mm3 BGO sample. The intrinsic LY and light loss coefficient were evaluated. The photofraction in pulse height spectrum of 662 keV γ-rays and the mass attenuation coefficient at 59.5 and 662 keV γ-rays were also determined and compared with the theoretical ones calculated using the WinXCom program.

Double-Diffusive Convection During Growth of Halides and Selenides

NASA Technical Reports Server (NTRS)

Singh, N. B.; Su, Ching-Hua; Duval, Walter M. B.

2015-01-01

Heavy metal halides and selenides have unique properties which make them excellent materials for chemical, biological and radiological sensors. Recently it has been shown that selenohalides are even better materials than halides or selenides for gamma-ray detection. These materials also meet the strong needs of a wide band imaging technology to cover ultra-violet (UV), midwave infrared wavelength (MWIR) to very long wavelength infrared (VLWIR) region for hyperspectral imager components such as etalon filters and acousto-optic tunable filters (AO). In fact AOTF based imagers based on these materials have some superiority than imagers based on liquid crystals, FTIR, Fabry-Perot, grating, etalon, electro-optic modulation, piezoelectric and several other concepts. For example, broadband spectral and imagers have problems of processing large amount of information during real-time observation. Acousto-Optic Tunable Filter (AOTF) imagers are being developed to fill the need of reducing processing time of data, low cost operation and key to achieving the goal of covering long-wave infrared (LWIR). At the present time spectral imaging systems are based on the use of diffraction gratings are typically used in a pushbroom or whiskbroom mode. They are mostly used in systems and acquire large amounts of hyperspectral data that is processed off-line later. In contrast, acousto-optic tunable filter spectral imagers require very little image processing, providing new strategies for object recognition and tracking. They are ideally suited for tactical situations requiring immediate real-time image processing. But the performance of these imagers depends on the quality and homogeneity of acousto-optic materials. In addition for many systems requirements are so demanding that crystals up to sizes of 10 cm length are desired. We have studied several selenides and halide crystals for laser and AO imagers for MWIR and LWIR wavelength regions. We have grown and fabricated crystals of several materials such as mercurous chloride, mercurous bromide, mercurous iodide, lead chloride lead bromide, lead iodide, thallium arsenic selenide, gallium selenide, zince sulfide zinc selenide and several crystals into devices. We have used both Bridgman and physical vapor transport (PVT) crystal growth methods. In the past have examined PVT growth numerically for conditions where the boundary of the enclosure is subjected to a nonlinear thermal profile. Since past few months we have been working on binary and ternary materials such as selenoiodides, doped zinc sulfides and mercurous chloro bromide and mercurous bromoiodides. In the doped and ternary materials thermal and solutal convection play extremely important role during the growth. Very commonly striations and banding is observed. Our experiments have indicated that even in highly purified source materials, homogeneity in 1-g environment is very difficult. Some of our previous numerical studies have indicated that gravity level less than 10-4 (?-g) helps in controlling the thermosolutal convection. We will discuss the ground based growth results of HgClxBr(1-x) and ZnSe growth results for the mm thick to large cm size crystals. These results will be compared with our microgravity experiments performed with this class of materials. For both HgCl-HgBr and ZnS-ZnSe the lattice parameters of the mixtures obey Vagard's law in the studied composition range. The study demonstrates that properties are very anisotropic with crystal orientation, and performance achievement requires extremely careful fabrication to utilize highest figure of merit. In addition, some parameters such as crystal growth fabrication, processing time, resolution, field of view and efficiency will be described based on novel solid solution materials. It was predicted that very similar to the pure compounds solid solutions also have very large anisotropy, and very precise oriented and homogeneous bulk and thin film crystals is required to achieve maximum performance of laser or imagers. Some of the parameters controlling the homogeneity such as thermos-solutal convection driven forces can be controlled in microgravity environments to utilize the benefits of these unique materials.

Crystal Chemical Controls on Equation of State

NASA Astrophysics Data System (ADS)

Thompson, R. M.; McCarthy, A. C.; Downs, R. T.

2007-12-01

Minerals are known to compress through a number of mechanisms, ranging from polyhedral distortion to electronic transitions. Two mechanisms which can produce significant volume decreases are angle-bending and bond compression. The crystal chemical effects of these two mechanisms have been studied and documented for years. With more recent advances in theory and software enabling the accurate determination of bonding topologies, M-O bonding to bridging oxygens has been shown to modify compressibility by changing angle-bending force constants. Minerals that compress mainly through angle-bending tend be soft. Good examples are quartz and cristobalite, minerals composed solely of corner-sharing silicate tetrahedra with bulk moduli of 37 and 12 GPa, respectively. Rock salt structured oxides must compress strictly by bond compression, and are much stiffer - lime and periclase have bulk moduli of 111 and 156 GPa, respectively. Feldspars have bulk moduli intermediate to the above examples. Based solely on the presence of Al-O-Si angles, theoretically softer than Si-O-Si angles, feldspars should be softer than quartz or cristobalite, but the T-O-T angles are stiffened by bonds to interstitial cations. The number and nature of these bonds affects compressibility sufficiently to create exceptions to Bridgman's law, which correlates bulk modulus with ambient unit cell volume in isostructural materials. In this paper, we present new high-pressure refinements of the crystal structures of jadeite, aegirine, and NaGa- clinopyroxene. Bulk moduli of these pyroxenes and all other end-member clinopyroxenes we could find in the literature (19 total) are plotted vs. unit cell volumes to test Bridgman's law. The data fall along two trends, each of which is separately consistent with Bridgman's law. Pyroxenes in one trend are dramatically stiffer than those in the other trend, with bulk moduli that differ by approximately 40 GPa. The only difference between the topologies of the structures in the two trends is in the bonding around M2. Structures in the less compressible trend have M2-O3 bonds that oppose Si-O-Si angle-bending in the tetrahedral chains. This angle-bending is an important compression mechanism in pyroxenes. McCarthy et al. (in press) term these bonds "antipathetic". Pyroxenes in the more compressible trend lack these bonds. There are other M2-O3 bonds that visual inspection suggests might tend to encourage angle-bending, but do not appear to have an effect. McCarthy et al. term these bonds "apathetic," and suggest the term "sympathetic" for M-O bonds that actually soften angles. Other examples from the literature will be presented including one from the feldspars that may be a truly sympathetic bond. McCarthy, A.C., Downs, R.T., and Thompson, R.M. (in press) Compressibility trends of the clinopyroxenes, and in- situ high-pressure single-crystal X-ray diffraction study of jadeite. American Mineralogist.

Defect, Kinetics and Heat Transfer of CDTE Bridgman Growth without Wall Contact

NASA Technical Reports Server (NTRS)

Larson, D. J., Jr.; Zhang, H.

2003-01-01

A detached growth mechanism has been proposed, which is similar to that proposed by Duffar et al. and used to study the current detached growth system. From numerical results, we can conclude that detached growth will more likely appear if the growth and wetting angles are large and meniscus is flat. Detached thickness is dependent on growth angle, wetting angle, and gap width and shape of the fins. The model can also explain why the detached growth will not happen for metals in which the growth angle is almost zero. Since the growth angle of CdZnTe cannot be changed, to promote detached growth, the number density of the fins should be low and the wetting angle should be high. Also, a much smaller gap width of the fins should be used in the ground experiment and the detached gap width is much smaller. The shape of the fins has minor influence on detached growth. An integrated numerical model for detached solidification has been developed combining a global heat transfer sub-model and a wall contact sub-model. The global heat transfer sub-model accounts for heat and mass transfer in the multiphase system, convection in the melt, macro-segregation, and interface dynamics. The location and dynamics of the solidification interface are accurately tracked by a multizone adaptive grid generation scheme. The wall contact sub-model accounts for the meniscus dynamics at the three-phase boundary. Simulations have been performed for crystal growth in a conventional ampoule and a designed ampoule to understand the benefits of detached solidification and its impacts on crystalline structural quality, e.g., stoichiometry, macro-segregation, and stress. From simulation results, both the Grashof and Marangoni numbers will have significant effects on the shape of growth front, Zn concentration distribution, and radial segregation. The integrated model can be used in designing apparatus and determining the optimal geometry for detached solidification in space and on the ground.

l en configuration dite de "Bridgman verticale" avec un tirage vers le haut. Pour des valeurs élevées du nombre de Rayleigh solutal, nous suivons les diverses branches de solutions stationnaires jusqu'aux seuils d'apparition des phénomènes instationnaires. Ces transitions à l'instationnarité sont étudiées en fonction du confinement et, le long de ces nouvelles branches de solution, nous estimons l'ordre de grandeur de la fluctuation temporelle de la composition à l'interface. Cette dernière étant responsable d'une striation qui est incorporée par le solide lors de sa croissance, nous caractérisons ce phénomène en termes d'amplitude de striation (i.e. intensité de la fluctuation de composition) et de période spatiale de striation.

NASA Astrophysics Data System (ADS)

Haldenwang, P.; Guérin, R.; Le Marec, C.

1999-06-01

2-D unsteady flow patterns in upward Bridgman solidification are numerically investigated. The alloy under study is Pb-30%Tl. The purpose of the contribution is to characterise the striations induced by unsteadiness in the growing crystal. Unsteady solution branches are studied from onset threshold of unsteadiness to chaos. We report two examples for which time behaviour of a given solution branch is studied versus Rayleigh number. We then estimate the magnitude of the time fluctuations in solute composition that the crystal incorporates. The period of the striations is also discussed. Nous étudions numériquement les structures hydrodynamiques de la convection solutale dans le bain fondu, lors de la solidification dirigée d'alliages binaires. Plus précisément, cette étude porte

Effect of modified mold shell on the microstructure and tensile fracture morphology of single-crystal nickel-base superalloy

NASA Astrophysics Data System (ADS)

Xu, Weitai; Zhao, Yutao; Sun, Shaochun; Liu, Manping; Ma, Dexin; Liang, Xiangfeng; Wang, Cunlong; Tao, Ran

2018-04-01

The mold shell used for single-crystal turbine blades preparation was modified from conventional process to fiber reinforcement technology. The wall thickness was decreased by 32.3 percent (pct) than the conventional process. Then these two mold shells were used to produce single crystal samples of nickel-base superalloy in a Bridgman furnace. The local temperature curves were recorded in the process. The results show that the modified mold shell can increase the temperature gradient in the mushy zone than the conventional mold shell. The primary and secondary dendrite arm space were reduced by 8 pct and 12 pct, respectively. Moreover, both the area fraction and mean size of the γ‧/γ eutectic were declined, as well as the dendritic segregation tendency. Therefore it contributed to the lower residual eutectic and micro-porosity in the heat-treated microstructure. Further, fracture surface of the samples made by modified mold shell exhibited smaller facets and more uniform dimples in the size and shape.

Multi-Layer SnSe Nanoflake Field-Effect Transistors with Low-Resistance Au Ohmic Contacts

NASA Astrophysics Data System (ADS)

Cho, Sang-Hyeok; Cho, Kwanghee; Park, No-Won; Park, Soonyong; Koh, Jung-Hyuk; Lee, Sang-Kwon

2017-05-01

We report p-type tin monoselenide (SnSe) single crystals, grown in double-sealed quartz ampoules using a modified Bridgman technique at 920 °C. X-ray powder diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX) measurements clearly confirm that the grown SnSe consists of single-crystal SnSe. Electrical transport of multi-layer SnSe nanoflakes, which were prepared by exfoliation from bulk single crystals, was conducted using back-gated field-effect transistor (FET) structures with Au and Ti contacts on SiO2/Si substrates, revealing that multi-layer SnSe nanoflakes exhibit p-type semiconductor characteristics owing to the Sn vacancies on the surfaces of SnSe nanoflakes. In addition, a strong carrier screening effect was observed in 70-90-nm-thick SnSe nanoflake FETs. Furthermore, the effect of the metal contacts to multi-layer SnSe nanoflake-based FETs is also discussed with two different metals, such as Ti/Au and Au contacts.

OSL studies of alkali fluoroperovskite single crystals for radiation dosimetry

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Raja, A.; Madhusoodanan, U.; Annalakshmi, O.; Ramasamy, P.

2016-08-01

This paper presents a preliminary investigation of the optically stimulated luminescence (OSL) of alkali fluoroperovskite single crystals for radiation dosimetry. The perovskite-like KMgF3, NaMgF3 and LiBaF3 polycrystalline compounds doped with rare earths (Eu2+ and Ce3+) were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of these compounds have been grown from melt by using vertical Bridgman-Stockbarger method. The Linearly Modulated OSL and Continuous Wave OSL measurements were performed in these alkali fluorides using blue light stimulation. Thermal bleaching experiments have shown that OSL signals originate from traps which are unstable near 200 °C, thus proving the suitability of the signals for dosimetric purposes. Optical bleaching measurements were also performed for these fluoride samples. OSL dose response was studied as a function of dose which was found to increase with beta dose.

Enhancement of thermoelectric figure of merit in β-Zn{sub 4}Sb{sub 3} by indium doping control

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

Wei, Pai-Chun, E-mail: pcwei68@gmail.com, E-mail: cheny2@phys.sinica.edu.tw; Hsu, Chia-Hao; Chang, Chung-Chieh

2015-09-21

We demonstrate the control of phase composition in Bridgman-grown β-Zn{sub 4}Sb{sub 3} crystals by indium doping, an effective way to overcome the difficulty of growing very pure β-Zn{sub 4}Sb{sub 3} thermoelectric material. The crystal structures are characterized by Rietveld refinement with synchrotron X-ray diffraction data. The results show an anisotropic lattice expansion in In-doped β-Zn{sub 4}Sb{sub 3} wherein the zinc atoms are partially substituted by indium ones at 36f site of R-3c symmetry. Through the elimination of ZnSb phase, all the three individual thermoelectric properties are simultaneously improved, i.e., increasing electrical conductivity and Seebeck coefficient while reducing thermal conductivity. Undermore » an optimal In concentration (x = 0.05), pure phase β-Zn{sub 4}Sb{sub 3} crystal can be obtained, which possesses a high figure of merit (ZT) of 1.4 at 700 K.« less

Excitation-Power Dependence of the Near Band-Edge PL Spectra of CdMnTe with High Mn Concentrations

NASA Astrophysics Data System (ADS)

Hwang, Younghun; Um, Youngho; Park, Hyoyeol

2011-12-01

Temperature and excitation power dependences of photoluminescence (PL) measurements were studied for the CdMnTe crystal grown by the vertical Bridgman method. The near band-edge and intra-Mn2+ emissions were investigated as a function of temperature. The observed band-edge peak of the PL spectrum showed a clear blue-shift with decreasing temperature. However, the peak energy of the intra-Mn2+ transition did not decrease monotonically with changing temperature, as can be seen above 70 K. With increasing the excitation power, the intensity of the emission peak was increased.

Dependences of the density of M 1- x R x F2 + x and R 1- y M y F3- y single crystals ( M = Ca, Sr, Ba, Cd, Pb; R means rare earth elements) on composition

NASA Astrophysics Data System (ADS)

Sorokin, N. I.; Krivandina, E. A.; Zhmurova, Z. I.

2013-11-01

The density of single crystals of nonstoichiometric phases Ba1 - x La x F2 + x (0 ≤ x ≤ 0.5) and Sr0.8La0.2 - x Lu x F2.2 (0 ≤ x ≤ 0.2) with the fluorite (CaF2) structure type and R 1 - y Sr y F3 - y ( R = Pr, Nd; 0 ≤ y ≤ 0.15) with the tysonite (LaF3) structure type has been measured. Single crystals were grown from a melt by the Bridgman method. The measured concentration dependences of single crystal density are linear. The interstitial and vacancy models of defect formation in the fluorite and tysonite phases, respectively, are confirmed. To implement the composition control of single crystals of superionic conductors M 1 - x R x F2 + x and R 1 - y M y F3 - y in practice, calibration graphs of X-ray density in the MF2- RF3 systems ( M = Ca, Sr, Ba, Cd, Pb; R = La-Lu, Y) are plotted.

{1 1 1} facet growth laws and grain competition during silicon crystallization

NASA Astrophysics Data System (ADS)

Stamelou, V.; Tsoutsouva, M. G.; Riberi-Béridot, T.; Reinhart, G.; Regula, G.; Baruchel, J.; Mangelinck-Noël, N.

2017-12-01

Directional solidification from mono-crystalline Si seeds having different orientations along the growth direction is studied. Due to the frequent twinning phenomenon, new grains soon nucleate during growth. The grain competition is then characterized in situ by imaging the dynamic evolution of the grain boundaries and of the corresponding grain boundary grooves that are formed at the solid-liquid interface. To perform this study, an experimental investigation based on Bridgman solidification technique coupled with in situ X-ray imaging is conducted in an original device: GaTSBI (Growth at high Temperature observed by X-ray Synchrotron Beam Imaging). Imaging characterisation techniques using X-ray synchrotron radiation at ESRF (European Synchrotron Radiation Facility, Grenoble, France) are applied during the solidification to study the growth dynamics. Facetted/facetted grain boundary grooves only are studied due to their importance in the grain competition because of their implication in the twinning mechanism. The maximum undercooling inside the groove is calculated from the groove depth knowing the local temperature gradient. Additionally, thanks to dynamic X-ray images, the global solid-liquid interface growth rate and the normal growth rate of the {1 1 1} facets existing at the grooves and at the edges are measured. From these measurements, experimental growth laws that correlate the normal velocity of the {1 1 1} facets with the maximum undercooling of the groove are extracted and compared to existing theoretical models. Finally, the experimental laws found for the contribution to the undercooling of the {1 1 1} facets are in good agreement with the theoretical model implying nucleation and growth eased by the presence of dislocations. Moreover, it is shown that, for the same growth parameters, the undercooling at the level of the facets (always lower than 1 K) is higher at the edges so that there is a higher probability of twin nucleation at the edges which is in agreement with the grain structure development characterised in the present experiments as well as in the literature.

TL and PL studies on cubic fluoroperovskite single crystal (KMgF3: Eu2+, Ce3+)

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Madhusoodanan, U.; Annalakshmi, O.; Ramasamy, P.

2014-04-01

The perovskite-like KMgF3 polycrystalline compounds were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of (0.2 mol% of EuF3 and CeF3) Co-doped KMgF3 have been grown from melt by using a vertical Bridgman-Stockbarger method. Thermoluminescence (TL) characteristics of KMgF3 samples doped with Eu2+ and Ce3+ have been studied after β-ray irradiation. At ambient conditions the photoluminescence spectra consisted of sharp line peaked of Eu2+ at 360 nm attributed to the f → f transition (6P7/2→8S7/2) could only be observed due to the energy transfer from Ce3+ to Eu2+.

Trace impurities analysis determined by neutron activation in the PbI 2 crystal semiconductor

NASA Astrophysics Data System (ADS)

Hamada, M. M.; Oliveira, I. B.; Armelin, M. J.; Mesquita, C. H.

2003-06-01

In this work, a methodology for impurity analysis of PbI 2 was studied to investigate the effectiveness of the purification. Commercial salts were purified by the multi passes zone refining and grown by the Bridgman method. To evaluate the purification efficiency, samples from the bottom, middle and upper sections of the ZR ingot were analyzed after 200, 300 and 500 purification passes, by measurements of the impurity concentrations, using the neutron activation analysis (NAA) technique. There was a significant reduction of the impurities according to the purification numbers. The reduction efficiency was different for each element, namely: Au>Mn>Co˜Ag>K˜Br. The impurity concentration of the crystals grown after 200, 300 and 500 passes and the PbI 2 starting material were analyzed by NAA and plasma optical emission spectroscopy.

Irradiation effect on luminescence properties of fluoroperovskite single crystal (LiBaF3:Eu2+)

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Madhusoodanan, U.; Nithya, R.; Ramasamy, P.

2014-03-01

Single crystals of pure and Eu2+ doped LiBaF3 have been grown from melt by using a vertical Bridgman-Stockbarger method. Effects induced by irradiation on europium doped LiBaF3 (lithium barium fluoride) single crystals were monitored by optical absorption, photoluminescence and thermoluminescence studies. The absorption bands of Eu2+ ions with peaks at 240, 290 and 320 nm were observed in the LiBaF3:Eu2+ crystal. Drastic increase in absorption was noted below 600 nm after gamma irradiation, which was dependent on the radiation dose. The additional absorption peak at around 570 nm was observed in irradiated crystal due to the ionization process Eu2+(-)e-→Eu3+. Photoluminescence of Eu2+ doped LiBaF3 single crystal shows sharp line peaked at ~359 nm and a broad band extending between 370 and 450 nm which shows a considerable reduction in Eu2+ PL intensity after gamma irradiation. Irradiated LiBaF3:Eu2+ sample has revealed three intense TL glow peaks at 128 °C (peak-1), 281 °C (peak-2) and 407 °C (peak-3). Activation energy (E) and frequency factor (s) of the latter two peaks were determined by various heating rate (VHR) method and graphical method.

Solute redistribution and constitutional supercooling effects in vertical Bridgman grown indium gallium antimonide by accelerated crucible rotation technique

NASA Astrophysics Data System (ADS)

Vogel, K. Juliet

The ternary alloy, InxGa1- xSb, is a compound semiconducting material of compositionally tunable bandgap (0.18 - 0.72 eV), making it desirable for use in photovoltaic, photodetector, and other opto-electronic devices in the infra-red regime. In the past, this material has proven to be difficult to synthesize in bulk due to the large phase separation between the constituent binaries. In this work, InxGa1-xSb has been grown in a state-of-the-art, computer-controlled system based on vertical Bridgman technique designed to allow crucible rotation during solidification of the material to reincorporate excess solute and improve material quality. Independent thermocouples allow for in situ monitoring and maintenance of the temperature to 0.2°C precision during crystal growth, reducing compositional inhomogeneities caused by temperature fluctuations. A series of experiments has been performed to evaluate the effect of accelerated crucible rotation technique (ACRT) on the structural quality and compositional homogeneity of bulk-grown InxGa 1-xSb for a starting melt composition of x = 0.25. A lowering rate of 3 mm/hr has been employed, for an overall cooling rate of 5.1°C/hr, which deliberately exceeds the threshold for constitutional supercooling. Scanning electron microscopy (SEM) has been performed on samples of In0.18Ga0.82Sb revealing a 92% percent reduction in micro-cracking with the application of ACRT when compared to synthesis performed without rotation. Furthermore; electron probe microscopy (EPMA) indicates an order of magnitude improvement in compositional homogeneity in the direction of growth with the use of ACRT. Micro-cracking and compositional homogeneity throughout cross-sections of InxGa1-xSb material also indicate areas of improved mixing during solidification, which can be compared to existing models of fluid flow exhibited in ACRT. The boule synthesized with ACRT shows a decrease in compositional deviation of 62% in the first-to-freeze areas of the sample, indicating suppression of supercooling in areas identified as Ekman flow regions. Results also demonstrate evidence of "dead-zones" in the ACRT mixing in the extreme center of the material, which confirms computational models of ACRT-induced fluid flow above the Ekman shear layer.

GaAs Substrates for High-Power Diode Lasers

NASA Astrophysics Data System (ADS)

Mueller, Georg; Berwian, Patrick; Buhrig, Eberhard; Weinert, Berndt

GaAs substrate crystals with low dislocation density (Etch-Pit Density (EPD) < 500,^-2) and Si-doping ( ~10^18,^-3) are required for the epitaxial production of high-power diode-lasers. Large-size wafers (= 3 mathrm{in} -> >=3,) are needed for reducing the manufacturing costs. These requirements can be fulfilled by the Vertical Bridgman (VB) and Vertical Gradient Freeze (VGF) techniques. For that purpose we have developed proper VB/VGF furnaces and optimized the thermal as well as the physico-chemical process conditions. This was strongly supported by extensive numerical process simulation. The modeling of the VGF furnaces and processes was made by using a new computer code called CrysVUN++, which was recently developed in the Crystal Growth Laboratory in Erlangen.GaAs crystals with diameters of 2 and 3in were grown in pyrolytic Boron Nitride (pBN) crucibles having a small-diameter seed section and a conical part. Boric oxide was used to fully encapsulate the crystal and the melt. An initial silicon content in the GaAs melt of c (melt) = 3 x10^19,^-3 has to be used in order to achieve a carrier concentration of n = (0.8- 2) x10^18,^-3, which is the substrate specification of the device manufacturer of the diode-laser. The EPD could be reduced to values between 500,^-2 and 50,^-2 with a Si-doping level of 8 x10^17 to 1 x10^18,^-3. Even the 3in wafers have rather large dislocation-free areas. The lowest EPDs ( <100,^-2) are achieved for long seed wells of the crucible.

Project Description and Publications List for UAH CMMR

NASA Technical Reports Server (NTRS)

Kaukler, William F.

1999-01-01

This research combines a state of the art X-ray Transmission Microscope, XTM, with a specially designed x-ray transparent horizontal Bridgman furnace to image (with resolutions up to 3 micrometers) the solidification of metal alloys in real-time. The objective is to obtain real-time dynamic data to provide direct measure of the solute profile in the liquid, phase coalescence and growth in the liquid, and the detailed interface morphology (e,g., dendrites and cells) during solidification. We are also enhancing the XTM data with precise solid-liquid interfacial temperature and the thermal gradient measurement techniques, and working on the application of this technology to the study of the fundamentals of solidification in microgravity. Over the last several years we have successfully imaged in real-time: interfacial-morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid. Interfacial undercoolings are being measured either with a special Seebeck furnace or with micro-thermocouple arrays we are developing. These later techniques are presently being incorporated with the XTM furnace. This last year emphasized the investigation of the solute layer in the melt during solidification. Methods were developed to quantify the solute concentrations using x-ray absorption and to compare to predictions from simulations. In addition, work is being completed on a brass-board portable XTM that incorporates a vertical Bridgman furnace.

Phase diagram and electrical behavior of silicon-rich iridium silicide compounds

NASA Technical Reports Server (NTRS)

Allevato, C. E.; Vining, Cronin B.

1992-01-01

The iridium-silicon phase diagram on the silicon-rich side was investigated by means of X-ray powder diffraction, density, differential thermal analysis, metalography, microprobe analysis, and electrical resistivity. Attempts were made to prepare eight previously reported silicon-rich iridium silicide compounds by arc melting and Bridgman-like growth. However, microprobe analysis identified only four distinct compositions: IrSi, Ir3Si4, Ir3Si5 and IrSi sub about 3. The existence of Ir4Si5 could not be confirmed in this study, even though the crystal structure has been previously reported. Differential thermal analysis (DTA) in conjunction with X-ray powder diffraction confirm polymorphism in IrSi sub about 3, determined to have orthorhombic and monoclinic unit cells in the high and low temperature forms. A eutectic composition alloy of 83 +/- 1 atomic percent silicon was observed between IrSi sub about 3 and silicon. Ir3Si4 exhibits distinct metallic behavior while Ir3Si5 is semiconducting. Both and IrSi and IrSi sub about 3 exhibit nearly temperature independent electrical resistivities on the order of 5-10 x 10 exp -6 ohms-m.

Synthesis, purification and bulk crystal growth of radiation detector materials using melt growth technique

NASA Astrophysics Data System (ADS)

Surabhi, Raja Rahul Reddy

In the past decade, there has been new and increased usage of radiation-detection technologies for applications in homeland security, non-proliferation, and national defense. Most of these applications require a portable device with high gamma-ray energy resolution and detection efficiency, compact size, room-temperature operation, and low cost. Consequently, there is a renewed understanding of the material limitations for these technologies and a great demand to develop next-generation radiation-detection materials that can operate at room temperature. Mercuric iodide (HgI2), Lead iodide (PbI2), and CdZnTe (CZT) are the current leading candidates for radiation detector applications. This is because of their high atomic number and large band gap that makes them particularly well suited for fabrication of high resolution and high efficiency compact devices. PbI2 is a promising material for room temperature nuclear radiation detectors, characterized by its wide band gap (EG=2.32eV) and high-density (rho=6.2g/cm3). It has been reported that PbI2 crystal detectors are able to detect gamma-ray in the range of 1KeV-1MeV, with good energy resolution. However, PbI 2 detectors have not been studied in detail because of non-availability of high quality single crystals. This study presents the synthesis, purification, growth and characterization of PbI2 single crystals grown. In this research, solid-state synthesis technique has been utilized for obtaining PbI2 as a starting material. For the first time, a unique low-temperature purification technique has been developed to obtain high-purity starting material. The crystals were grown using 2-zone Bridgman-Stockbarger (B.S) technique wherein growth rate and temperature gradient at the solid-liquid interface were optimized. Single crystals of PbI2 were successfully grown in quartz glass ampoule under different growth conditions. Material purity was determined by measuring the elemental concentration using the Inductively coupled plasma-optical emission spectroscopy (ICP-OES). ICP-OES is utilized for estimating impurities present in the low-temperature purified material, zone refined material and melt grown PbI2 crystals. The zone-refined material contains no traceable amounts of impurities, whereas the low-temperature purified material and melt grown PbI2 crystals show very low concentration of K (potassium) and Na (sodium) impurities. Crystal characterization has been performed for determining optical properties by UV-VIS spectroscopy. The energy band gap (EG) is an important parameter for materials used for room temperature gamma-ray detector applications. The absorption peak at 530nm is a characteristic of PbI2 and corresponds to the onset of the transitions from the valence band to the exciton level. From this absorption spectrum the calculated indirect band gap of PbI 2 was 2.33+/-0.025 eV at room temperature. For measuring the electrical properties (Dielectric and I-V characteristics) of the crystal, Ag (silver) contacts are applied to both sides of the sample. Dielectric analysis on melt grown PbI2 showed that space charge polarization was dominant at lower frequencies but stabilizes at higher frequencies over different operating temperatures. On the other hand, dielectric analysis for zone-refined material space charge polarization was constant over the operating range resulting in fewer lattice defects. Therefore the low temperature purified material followed by zone-refined purification provides detector grade material with fewer lattice defects. The measured electrical resistivity for melt grown PbI2 and zone-refined material are 3.185 x 10 10 O-cm and 0.754 x 109 O-cm at room temperature along (001) plane respectively.

Defect levels of semi-insulating CdMnTe:In crystals

NASA Astrophysics Data System (ADS)

Kim, K. H.; Bolotinikov, A. E.; Camarda, G. S.; Hossain, A.; Gul, R.; Yang, G.; Cui, Y.; Prochazka, J.; Franc, J.; Hong, J.; James, R. B.

2011-06-01

Using photoluminescence (PL) and current deep-level transient spectroscopy (I-DLTS), we investigated the electronic defects of indium-doped detector-grade CdMnTe:In (CMT:In) crystals grown by the vertical Bridgman method. We similarly analyzed CdZnTe:In (CZT:In) and undoped CdMnTe (CMT) crystals grown under the amount of same level of excess Te and/or indium doping level to detail the fundamental properties of the electronic defect structure more readily. Extended defects, existing in all the samples, were revealed by synchrotron white beam x-ray diffraction topography and scanning electron microscopy. The electronic structure of CMT is very similar to that of CZT, with shallow traps, A-centers, Cd vacancies, deep levels, and Te antisites. The 1.1-eV deep level, revealed by PL in earlier studies of CZT and CdTe, were attributed to dislocation-induced defects. In our I-DLTS measurements, the 1.1-eV traps showed different activation energies with applied bias voltage and an exponential dependence on the trap-filling time, which are typical characteristics of dislocation-induced defects. We propose a new defect-trap model for indium-doped CMT crystals.

Luminescence properties of Eu3+ doped CdF2 single crystals

NASA Astrophysics Data System (ADS)

Boubekri, H.; Diaf, M.; Guerbous, L.; Jouart, J. P.

2018-04-01

This paper reports the photoluminescence properties of Eu3+ doped CdF2 single crystals. The pulled crystals were prepared by use of the Bridgman technique from a vacuum furnace in fluoride atmosphere. Absorption, excitation and emission spectra of the crystal doped with three Eu3+ concentrations (0.02%, 0.1% and 0.6% mol.) were recorded at room temperature. The emission spectra exhibit a strong yellow and red emissions in the spectral range 550-720 nm which are assigned to 5D0 → 7FJ (J = 1, 2, 4) transitions and a weak infrared emission around 816 nm corresponding to 5D0 → 7F6 transition. The magnetic dipole emission (5D0 → 7F1) is the most intense for each Eu3+ concentration. The Judd-Ofelt intensity parameters Ω2, Ω4, Ω6 for 4f-4f transitions of Eu3+ ions were computed from the emission spectra using the 5D0 → 7FJ (J = 1, 2, 4, 6) transitions. Via these phenomenological intensity parameters, the spontaneous emission probabilities, branching ratios, radiative lifetimes, quantum efficiencies and emission cross-sections for the main Eu3+ emitting levels are evaluated.

Scintillation properties of the silver doped lithium iodide single crystals at room and low temperature

NASA Astrophysics Data System (ADS)

Khan, Sajid; Kim, H. J.; Lee, M. H.

2016-06-01

This study presents luminescence and scintillation properties of Silver doped LiI crystals. Single crystals of LiI: x% Ag (x=0.02, 0.05, 0.1 and 0.5) were grown by using the Bridgman technique. X-ray induced luminescence spectra show emission bands spanning from 275 nm to 675 nm, dominated by Ag+ band having a peak at 300 nm. Under UV-luminescence, a similar emission band was observed with the peak excitation wavelength of 265 nm. Energy resolution, light yield and decay time profiles of the samples were measured under a 137Cs γ-ray irradiation. The LiI(0.1%Ag) showed the highest light yield and the best energy resolution among the samples. The light yield of LiI(0.1%Ag) is higher than commercially available LiI(Eu) crystal (15,000±1500 ph/MeV). The LiI(Ag) samples exhibit three exponential decay time components except the LiI(0.02%Ag), where the fitting found two decay time components. Temperature dependences of emission spectra, light yield and decay time were studied from 300 K to 10 K. The LiI(0.1%Ag) crystal showed an increase in the light yield and a shortening of decay time with a decrease in temperature..

High-efficiency thermoelectric Ba8Cu14Ge6P26: bridging the gap between tetrel-based and tetrel-free clathrates† †Electronic supplementary information (ESI) available: Calculated and experimental powder XRD patterns; tables with crystallographic information; SEM and EDS results; additional DSC, thermal conductivities, and ZT figures. CCDC 1568106. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c7sc03482b

PubMed Central

Wang, Jian; Lebedev, Oleg I.; Lee, Kathleen; Dolyniuk, Juli-Anna; Klavins, Peter; Bux, Sabah

2017-01-01

A new type-I clathrate, Ba8Cu14Ge6P26, was synthesized by solid-state methods as a polycrystalline powder and grown as a cm-sized single crystal via the vertical Bridgman method. Single-crystal and powder X-ray diffraction show that Ba8Cu14Ge6P26 crystallizes in the cubic space group Pm3n (no. 223). Ba8Cu14Ge6P26 is the first representative of anionic clathrates whose framework is composed of three atom types of very different chemical natures: a transition metal, tetrel element, and pnicogen. Uniform distribution of the Cu, Ge, and P atoms over the framework sites and the absence of any superstructural or local ordering in Ba8Cu14Ge6P26 were confirmed by synchrotron X-ray diffraction, electron diffraction and high-angle annular dark field scanning transmission electron microscopy, and neutron and X-ray pair distribution function analyses. Characterization of the transport properties demonstrate that Ba8Cu14Ge6P26 is a p-type semiconductor with an intrinsically low thermal conductivity of 0.72 W m–1 K–1 at 812 K. The thermoelectric figure of merit, ZT, for a slice of the Bridgman-grown crystal of Ba8Cu14Ge6P26 approaches 0.63 at 812 K due to a high power factor of 5.62 μW cm–1 K–2. The thermoelectric efficiency of Ba8Cu14Ge6P26 is on par with the best optimized p-type Ge-based clathrates and outperforms the majority of clathrates in the 700–850 K temperature region, including all tetrel-free clathrates. Ba8Cu14Ge6P26 expands clathrate chemistry by bridging conventional tetrel-based and tetrel-free clathrates. Advanced transport properties, in combination with earth-abundant framework elements and congruent melting make Ba8Cu14Ge6P26 a strong candidate as a novel and efficient thermoelectric material. PMID:29568451

Separation of CsCl from a Ternary CsCl-LiCl-KCl Salt via a Melt Crystallization Technique for Pyroprocessing Waste Minimization

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

Ammon Williams; Supathorn Phongikaroon; Michael Simpson

A parametric study has been conducted to identify the effects of several parameters on the separation of CsCl from molten LiCl-KCl salt via a melt crystallization process. A reverse vertical Bridgman technique was used to grow the salt crystals. The investigated parameters were: (1) the advancement rate, (2) the crucible lid configuration, (3) the amount of salt mixture, (4) the initial composition of CsCl, and (5) the temperature difference between the high and low furnace zones. From each grown crystal, samples were taken axially and analyzed using inductively coupled plasma mass spectrometry (ICP-MS). Results show that CsCl concentrations at themore » top of the crystals were low and increased to a maximum at the bottom of the salt. Salt (LiCl-KCl) recycle percentages for the experiments ranged from 50% to 75% and the CsCl composition in the waste salt was low. To increase the recycle percentage and the concentration of CsCl in the waste form, the possibility of using multiple crystallization stages was explored to further optimize the process. Results show that multiple crystallization stages are practical and the optimal experimental conditions should be operated at 5.0 mm/hr rate with a lid configuration and temperature difference of 200 °C for a total of five crystallization stages. Under these conditions, up to 88% of the salt can be recycled.« less

Bulk Crystal Growth, and High-Resolution X-ray Diffraction Results of LiZnAs Semiconductor Material

NASA Astrophysics Data System (ADS)

Montag, Benjamin W.; Reichenberger, Michael A.; Sunder, Madhana; Ugorowski, Philip B.; Nelson, Kyle A.; Henson, Luke C.; McGregor, Douglas S.

2017-08-01

LiZnAs is being explored as a candidate for solid-state neutron detectors. The compact form, solid-state device would have greater efficiency than present day gas-filled 3He and 10BF3 detectors. Devices fabricated from LiZnAs having either natural Li (nominally 7.5% 6Li) or enriched 6Li (usually 95% 6Li) as constituent atoms may provide a material for compact high efficiency neutron detectors. The 6Li( n, t)4He reaction yields a total Q-value of 4.78 MeV, an energy larger than that of the 10B reaction, which can easily be identified above background radiations. LiZnAs material was synthesized by preparing equimolar portions of Li, Zn, and As sealed under vacuum (10-6 Torr) in quartz ampoules lined with boron nitride and subsequently reacted in a compounding furnace (Montag et al. in J Cryst Growth 412:103, 2015). The raw synthesized LiZnAs was purified by a static vacuum sublimation in quartz (Montag et al. in J Cryst Growth 438:99, 2016). Bulk crystalline LiZnAs ingots were grown from the purified material with a high-temperature Bridgman-style growth process described here. One of the largest LiZnAs ingots harvested was 9.6 mm in diameter and 4.2 mm in length. Samples were harvested from the ingot and were characterized for crystallinity using a Bruker AXS Inc. D8 AXS Inc. D2 CRYSO, energy dispersive x-ray diffractometer, and a Bruker AXS Inc. D8 DISCOVER, high-resolution x-ray diffractometer equipped with molybdenum radiation, Gobel mirror, four bounce germanium monochromator and a scintillation detector. The primary beam divergence was determined to be 0.004°, using a single crystal Si standard. The x-ray based characterization revealed that the samples nucleated in the (110) direction and a high-resolution open detector rocking curve recorded on the (220) LiZnAs yielded a full width at half maximum (FWHM) of 0.235°. Sectional pole figures using off-axis reflections of the (211) LiZnAs confirmed in-plane ordering, and also indicated the presence of multiple domains. The LiZnAs bulk crystals exhibited a Primitive Cubic Bravais lattice instead of the commonly reported Face-centered Cubic Bravais lattice. The lattice constant was determined to be 5.5146 ± 0.0003 Å.

Energy transfer and 2.0 μm emission in Tm{sup 3+}/Ho{sup 3+} co-doped α-NaYF{sub 4} single crystals

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

Feng, Zhigang; Yang, Shuo; Xia, Haiping, E-mail: hpxcm@nbu.edu.cn

2016-04-15

Highlights: • Cubic NaYF{sub 4} single crystals co-doped with ∼1.90 mol% Tm{sup 3+} and various Ho{sup 3+} concentrations were grown by Bridgman method. • The maximum fluorescence lifetime was 23.23 ms for Tm{sup 3+} (1.90 mol%)/Ho{sup 3+} (3.89 mol%) co-doped α-NaYF{sub 4}. • The obtained energy transfer rate (W{sub ET}) and energy transfer efficiency (η) of Tm{sup 3+}:{sup 3}F{sub 4} are 1077 s{sup −1} and 95.0%, respectively. • The maximum emission cross section reached 1.06 × 10{sup −20} cm{sup 2}. - Abstract: Cubic NaYF{sub 4} single crystals co-doped with ∼1.90 mol% Tm{sup 3+} and various Ho{sup 3+} concentrations were grownmore » by Bridgman method. The energy transfer from Tm{sup 3+} to Ho{sup 3+} and the optimum fluorescence emission around 2.04 μm of Ho{sup 3+} ion were investigated based on the measured absorption spectra, emission spectra, emission cross section and decay curves under excitation of 800 nm LD. The emission intensity at 2.04 μm increased with the increase of Ho{sup 3+} concentration from 0.96 mol% to 3.89 mol% when the concentration of Tm{sup 3+} was held constantly at ∼1.90 mol%. Moreover, the maximum emission cross section reached 1.06 × 10{sup −20} cm{sup 2} and the maximum fluorescence lifetime was 23.23 ms for Tm{sup 3+}(1.90 mol%)/Ho{sup 3+}(3.89 mol%) co-doped one. According to the measured lifetime of Tm{sup 3+} single-doped and Tm{sup 3+}/Ho{sup 3+} co-doped samples, the maximum energy transfer efficiency of Tm{sup 3+}:{sup 3}F{sub 4} level was 95.0%. Analysis on the fluorescence dynamics indicated that electric dipole–dipole is dominant for the energy transfer from Tm{sup 3+} to Ho{sup 3+}.« less

Transport processes in directional solidification and their effects on microstructure development

NASA Astrophysics Data System (ADS)

Mazumder, Prantik

The processing of materials with unique electronic, mechanical, optical and thermal properties plays a crucial role in modern technology. The quality of these materials depend strongly on the microstructures and the solute/dopant fields in the solid product, that are strongly influenced by the intricate coupling of heat and mass transfer and melt flow in the growth systems. An integrated research program is developed that include precisely characterized experiments and detailed physical and numerical modeling of the complex transport and dynamical processes. Direct numerical simulation of the solidification process is carried out that takes into account the unsteady thermo-solutal convection in the vertical Bridgman crystal growth system, and accurately models the thermal interaction between the furnace and the ampoule by appropriately using experimentally measured thermal profiles. The flow instabilities and transitions and the nonlinear evolution following the transitions are investigated by time series and flow pattern analysis. A range of complex dynamical behavior is predicted with increasing thermal Rayleigh number. The route to chaos appears as: steady convection --> transient mono-periodic --> transient bi-periodic --> transient quasiperiodic --> transient intermittent oscillation- relaxation --> stable intermittent oscillation-relaxation attractor. The spatio-temporal dynamics of the melt flow is found to be directly related to the spatial patterns observed experimentally in the solidified crystals. The application of the model to two phase Sn-Cd peritectic alloys showed that a new class of tree-like oscillating microstructure develops in the solid phase due to unsteady thermo-solutal convection in the liquid melt. These oscillating layered structures can give the illusion of band structures on a plane of polish. The model is applied to single phase solidification in the Al-Cu and Pb-Sn systems to characterize the effect of convection on the macroscopic shape and disorder in the primary arm spacing of the cellular/dendritic freezing front. The apparently puzzling experimental observation of higher disorder in the weakly convective Al-Cu system than that in the highly convective Pb-Sn system is explained by the numerical calculations.

Dependences of the density of M{sub 1-x}R{sub x}F{sub 2+x} and R{sub 1-y}M{sub y}F{sub 3-y} single crystals (M = Ca, Sr, Ba, Cd, Pb; R means rare earth elements) on composition

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

Sorokin, N. I., E-mail: sorokin@ns.crys.ras.ru; Krivandina, E. A.; Zhmurova, Z. I.

2013-11-15

The density of single crystals of nonstoichiometric phases Ba{sub 1-x}La{sub x}F{sub 2+x} (0 {<=} x {<=} 0.5) and Sr{sub 0.8}La{sub 0.2-x}Lu{sub x}F{sub 2.2} (0 {<=} x {<=} 0.2) with the fluorite (CaF{sub 2}) structure type and R{sub 1-y}Sr{sub y}F{sub 3-y} (R = Pr, Nd; 0 {<=} y {<=} 0.15) with the tysonite (LaF{sub 3}) structure type has been measured. Single crystals were grown from a melt by the Bridgman method. The measured concentration dependences of single crystal density are linear. The interstitial and vacancy models of defect formation in the fluorite and tysonite phases, respectively, are confirmed. To implement themore » composition control of single crystals of superionic conductors M{sub 1-x}R{sub x}F{sub 2+x} and R{sub 1-y}M{sub y}F{sub 3-y} in practice, calibration graphs of X-ray density in the MF{sub 2}-RF{sub 3} systems (M = Ca, Sr, Ba, Cd, Pb; R = La-Lu, Y) are plotted.« less

Current response of a TlBr detector to {sup 137}Cs {gamma}-ray radiation

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

Gazizov, I. M., E-mail: gazizov@isotop.dubna.ru; Zaletin, V. M.; Kukushkin, V. M.

2011-05-15

The current response of a TlBr detector to {sup 137}Cs {gamma}-ray radiation has been studied in the dose-rate range 0.033-3.84 Gy/min and within the voltage range 1-300 V; the detectors are based on pure and doped TlBr crystals grown from the melt by the Bridgman-Stockbarger method. The mass fraction of Pb or Ca introduced into the TlBr crystals was 1-10 ppm for Pb and 150 ppm for Ca. The current response of nominally undoped TlBr samples was nearly linear over two decades of studied dose rates. Deep hole levels associated with cationic vacancies V{sub c}{sup -} determine the dependence ofmore » the current response on the voltage in the high electric fields. The parameters of the carriers' transport {mu}{tau} are determined. The TlBr crystals grown in vacuum and in the bromine vapor exhibit a large mobility-lifetime product of 4.3 Multiplication-Sign 10{sup -4} and 6.4 Multiplication-Sign 10{sup -5} cm{sup 2}V{sup -1}, respectively. The value of {mu}{tau} is in the range (4-9) Multiplication-Sign 10{sup -5} cm{sup 2}V{sup -1} for crystals doped with a divalent cation.« less

Progress in the Development of the Lead Tungstate Crystals for EM-Calorimetry in High-Energy Physics

NASA Astrophysics Data System (ADS)

Novotny, R. W.; Brinkmann, K.-T.; Borisevich, A.; Dormenev, V.; Houzvicka, J.; Korjik, M.; Zaunick, H.-G.

2017-11-01

Even at present time there is a strong interest and demand for high quality lead tungstate crystals (PbWO4, PWO) for electromagnetic (EM) calorimetry. PWO is implemented into the EM calorimeter of the CMS-ECAL detector at LHC [1] and required for the completion of the PANDA EMC [2] and various ongoing detector projects at Jefferson Lab. The successful mass production of PWO using the Czochralski method was stopped after bankruptcy of the Bogoroditsk Technical Chemical Plant (BTCP) in Russia as major producer so far. The Shanghai Institute of Ceramics, Chinese Academy of Science (China) was considered as an alternative producer using the modified Bridgman method. The company CRYTUR (Turnov, Czech Republic) with good experience in the development and production of different types of inorganic oxide crystals has restarted at the end of 2014 the development of lead tungstate for mass production based on the Czochralski method. An impressive progress was achieved since then. The growing technology was optimized to produce full size samples with the quality meeting the PANDA-EMC specifications for PWO-II. We will present a detailed progress report on the research program in collaboration with groups at Orsay and JLab. The full size crystals will be characterized with respect to optical performance, light yield, kinetics and radiation hardness.

TL and PL studies on cubic fluoroperovskite single crystal (KMgF{sub 3}: Eu{sup 2+}, Ce{sup 3+})

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

Daniel, D. Joseph, E-mail: josephd@ssn.edu.in; Ramasamy, P.; Madhusoodanan, U.

2014-04-24

The perovskite-like KMgF{sub 3} polycrystalline compounds were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of (0.2 mol% of EuF{sub 3} and CeF{sub 3}) Co-doped KMgF{sub 3} have been grown from melt by using a vertical Bridgman-Stockbarger method. Thermoluminescence (TL) characteristics of KMgF{sub 3} samples doped with Eu{sub 2+} and Ce{sub 3+} have been studied after β-ray irradiation. At ambient conditions the photoluminescence spectra consisted of sharp line peaked of Eu{sub 2+} at 360 nm attributed to the f → f transition ({sup 6}P{sub 7/2}→{sup 8}S{submore » 7/2}) could only be observed due to the energy transfer from Ce{sub 3+} to Eu{sub 2+}.« less

Jahn-Teller effect on the [TiF 4F 4F int] 6-(C 4v) and [NiF 4F 4F int] 7-(C 4v) clusters embedded into SrF 2 crystals

NASA Astrophysics Data System (ADS)

Ulanov, V. A.; Zhiteitcev, E. R.; Varlamov, A. G.

2007-07-01

By means of EPR method the associative [TiF 4F 4F int] 6-(C 4v) and [NiF 4F 4F int] 7-(C 4v) centers were revealed in the fluorite type SrF 2:Ti and SrF 2:Ni crystals grown by Bridgman method in helium atmosphere containing some amount of a fluorine gas. It was found that at low temperatures the local structures of these associative centers were exposed to a static rhombic distortion. The reasons of such distortions were accounted for by the assumption that the E ⊗ ( b1 + b2) vibronic interaction became effective due to that the ground orbital states of the [TiF 4F 4F int] 6-(C 4v) and [NiF 4F 4F int] 7-(C 4v) centers occurred to be doubly degenerated.

Stoichiometric Effects on the Photoelectric Properties of LiInSe 2 Crystals for Neutron Detection

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

Guo, Lijian; Xu, Yadong; Zheng, Hongjian

6LiInSe 2 is a promising semiconductor candidate for thermal neutron detection due to its large capture cross-section. However, the charge collection efficiency is still insufficient for high resolution for the grown-in defects induced by the stoichiometric deviation. In this work, we report photoelectric properties of stoichiometric LiInSe 2 crystal boules up to 70 mm in length and 20 mm in diameter grown by the vertical Bridgman method. Inductively coupled plasma measurements demonstrate that the ratio of Li, In, and Se of the as-grown crystal is very close to 1:1:2, which is optimized by low temperature synthesis processing. The obtained singlemore » crystals display high bulk resistivity in the range of 10 11–10 12 Ω·cm and a direct band gap of 2.01–2.83 eV with a changeable color from red to yellow. The electronic structure of LiInSe 2 was studied using first-principles density functional theory calculations, which predicts that the antisite defects of In Li and Li In are the dominant factor for the different crystal colors observed. The stoichiometric LiInSe 2 crystal gives an improved energy resolution, for a semiconductor detector when illuminated with a 241Am@5.48 MeV α source, of 23.3%. In conclusion, the electron mobility-lifetime product (μτ) is ~2.5 × 10 –5 cm 2 V –1.« less

Stoichiometric Effects on the Photoelectric Properties of LiInSe 2 Crystals for Neutron Detection

DOE PAGES

Guo, Lijian; Xu, Yadong; Zheng, Hongjian; ...

2018-04-16

6LiInSe 2 is a promising semiconductor candidate for thermal neutron detection due to its large capture cross-section. However, the charge collection efficiency is still insufficient for high resolution for the grown-in defects induced by the stoichiometric deviation. In this work, we report photoelectric properties of stoichiometric LiInSe 2 crystal boules up to 70 mm in length and 20 mm in diameter grown by the vertical Bridgman method. Inductively coupled plasma measurements demonstrate that the ratio of Li, In, and Se of the as-grown crystal is very close to 1:1:2, which is optimized by low temperature synthesis processing. The obtained singlemore » crystals display high bulk resistivity in the range of 10 11–10 12 Ω·cm and a direct band gap of 2.01–2.83 eV with a changeable color from red to yellow. The electronic structure of LiInSe 2 was studied using first-principles density functional theory calculations, which predicts that the antisite defects of In Li and Li In are the dominant factor for the different crystal colors observed. The stoichiometric LiInSe 2 crystal gives an improved energy resolution, for a semiconductor detector when illuminated with a 241Am@5.48 MeV α source, of 23.3%. In conclusion, the electron mobility-lifetime product (μτ) is ~2.5 × 10 –5 cm 2 V –1.« less

Characteristics of dielectric properties and conduction mechanism of TlInS2:Cu single crystals

NASA Astrophysics Data System (ADS)

El-Nahass, M. M.; Ali, H. A. M.; El-Zaidia, E. F. M.

2013-12-01

Single crystals of TlInS2:Cu were grown by the modified Bridgman method. The dielectric behavior of TlInS2:Cu was investigated using the impedance spectroscopy technique. The real (ε1), imaginary (ε2) parts of complex dielectric permittivity and ac conductivity were measured in the frequency range (42-2×105) Hz with a variation of temperature in the range from 291 K to 483 K. The impedance data were presented in Nyquist diagrams for different temperatures. The frequency dependence of σtot (ω) follows the Jonscher's universal dynamic law with the relation σtot (ω)=σdc+Aωs, (where s is the frequency exponent). The mechanism of the ac charge transport across the layers of TlInS2:Cu single crystals was referred to the hopping over localized states near the Fermi level. The examined system exhibits temperature dependence of σac (ω), which showed a linear increase with the increase in temperature at different frequencies. Some parameters were calculated as: the density of localized states near the Fermi level, NF, the average time of charge carrier hopping between localized states, τ, and the average hopping distance, R.

Quench hardening of Sb0.2 Bi1.8Te3, Bi2Te2.8Se0.2 and Sn0.2 Bi1.8Te3 single crystals

NASA Astrophysics Data System (ADS)

Soni, P. H.

2018-02-01

The V2-VI3 intermetallics are narrow band gap semiconductors and well known for their thermoelectric properties. They therefore offer a convenient route to tune band gap for manipulating thermoelectric parameters. The V group element Sb can be fruitfully used to substitute Bi in various proportions thus forming a psuedobinary solid solution. The electronic in general and the thermoelectric properties in particular of this psuedobinary have been amply reported. However there are no reports found on mechanical properties. I have used Sb0.2 Bi1.8Te3, Bi2Te2.8Se0.2 and Sn0.2 Bi1.8Te3single crystals grown using Bridgman technique for the quenching treatment followed by hardness testing. Vickers hardness tests were conducted on the cleavage planes of the crystals quenched from various high temperatures and the quench hardenening coefficient values have been determined. The hardness tests were carried out at various applied loads also to explore load dependence of the measured hardness. The results are reported in the paper.

Excited States of the A and B Free Excitons in CuInSe2

NASA Astrophysics Data System (ADS)

Yakushev, Michael V.; Luckert, Franziska; Faugeras, Clement; Karotki, Anatoli V.; Mudryi, Alexander V.; Martin, Robert W.

2011-05-01

CuInSe2 single crystals, grown by the vertical Bridgman technique were studied using polarisation resolved photoluminescence (PL) at cryogenic temperatures. The emission lines related to the first (n = 2) excited states for the A and B free excitons were observed in the PL spectra at 1.0481 and 1.0516 eV, respectively. The spectral positions of these lines were used to estimate accurate values for the A and B exciton binding energies (8.5 and 8.4 meV, respectively), Bohr radii (7.5 nm), band gaps (EgA = 1.050 eV and EgB = 1.054 eV), and the static dielectric constant (11.3) assuming the hydrogenic model.

Study on the effect of Cd-diffusion annealing on the electrical properties of CdZnTe

NASA Astrophysics Data System (ADS)

Wanwan, Li; Zechun, Cao; Bin, Zhang; Feng, Zhan; Hongtao, Liu; Wenbin, Sang; Jiahua, Min; Kang, Sun

2006-06-01

In order to meet the requirements for the device design of radiation detectors, CdZnTe (or Cd 1-xZn xTe) crystals grown by Vertical Bridgman Method often need subsequent annealing to increase their resistivity. The nature of this treatment is a diffusion process. Thus, it is meaningful to relate the change of resistivity to the diffusion parameters. A model correlating resistivity and conduction type of CdZnTe with the main diffusion parameter—diffusion coefficient—is put forward in this paper. Combining the model with the analysis of our experimental data, DCd=1.464×10 -10, 1.085×10 -11 and 4.167×10 -13 cm 2/s are the values of Cd self-diffusion coefficient in Cd 0.9Zn 0.1Te at 1073, 973 and 873 K, respectively. The data coincide closely with the Cd self-diffusion coefficient in CdTe provided by different authors [E.D. Jones, N.M. Stewart, Self-diffusion of cadmium in cadmium telluride, J. Crystal Growth 84 (1987) 289-294; P.M. Borsenberger, D.A. Stevenson, J. Phys. Chem. Solids 29 (1968) 1277; R.C. Whelan, D. Shaw, in: D.G. Thomas (Ed.), II -VI Semiconductor Compounds, Benjamin, New York, 1967, p. 451]. With the data, the effects of annealing time on the change of resistivity and conduction type for Cd 0.9Zn 0.1Te wafers, which are annealed in saturated Cd vapor at 1073, 973 and 873 K, were simulated, and good consistency was found. This work suggests an alternative way to obtain the diffusion coefficient in semiconductor materials and also enables ones to analyze the diffusion process quantitatively and predict the annealing results.

Crystal growth and structure, electrical, and optical characterization of the semiconductor Cu2SnSe3

NASA Astrophysics Data System (ADS)

Marcano, G.; Rincón, C.; de Chalbaud, L. M.; Bracho, D. B.; Pérez, G. Sánchez

2001-08-01

X-ray powder diffraction by p-type Cu2SnSe3, prepared by the vertical Bridgman-Stockbarger technique, shows that this material crystallizes in a monoclinic structure, space group Cc, with unit cell parameters a=6.5936(1) Å, b=12.1593(4) Å, c=6.6084(3) Å, and β=108.56(2)°. The temperature variation of the hole concentration p obtained from the Hall effect and electrical resistivity measurements from about 160 to 300 K, is explained as due to the thermal activation of an acceptor level with an ionization energy of 0.067 eV, whereas below 100 K, the conduction in the impurity band dominates the electrical transport process. From the analysis of the p vs T data, the density-of-states effective mass of the holes is estimated to be nearly of the same magnitude as the free electron mass. In the valence band, the temperature variation of the hole mobility is analyzed by taking into account the scattering of charge carriers by ionized and neutral impurities, and acoustic phonons. In the impurity band, the mobility is explained as due to the thermally activated hopping transport. From the analysis of the optical absorption spectra at room temperature, the fundamental energy gap was determined to be 0.843 eV. The photoconductivity spectra show the presence of a narrow band gap whose main peak is observed at 0.771 eV. This band is attributed to a free-to-bound transition from the defect acceptor level to the conduction band. The origin of this acceptor state, consistent with the chemical composition of the samples and screening effects, is tentatively attributed to selenium interstitials.

Heat flow control and segregation in directional solidification: Development of an experimental and theoretical basis for Bridgman-type growth experiments in a microgravity environment

NASA Technical Reports Server (NTRS)

Witt, A. F.

1986-01-01

Within the framework of the proposed research, emphasis was placed on application of magnetic fields to semiconductor growth systems. It was found that magnetic fields up to 3 kGauss do not affect the growth behavior nor the macro-segregation behavior in the system Ge(Ga). Applied fields are found to significantlty alter the radial dopant distribution, which is attributed to alterations in the spatial orientation of convective cells. Increasing the magnetic field to 30 kGauss is found to have a fundamental effect on dopant segregation. Emphasis is also placed on the potential of KC-135 flights for preliminary studies on the effects of reduced gravity environments on the wetting behavior of semiconductor systems in growth configuration. The limited number of experiments conducted does not allow any conclusions on the merits of KC-135 flights for semiconductor processing research.

The Ni and Co substitutions in iron chalcogenide single crystals

NASA Astrophysics Data System (ADS)

Bezusyy, V. L.; Gawryluk, D. J.; Malinowski, A.; Berkowski, M.; Cieplak, Marta Z.

2015-03-01

We study the ab-plane resistivity and Hall effect in Fe1-yMyTe0.65Se0.35 single crystals with M =Co or Ni, and y up to 0.2. The crystals are grown by Bridgman's method. The low-temperature Hall coefficient RH changes sign to negative for crystals with y exceeding 0.135 (Co) and 0.06 (Ni), consistent with the electron doping induced by these impurities. However, the RH remains positive for all samples at high T, suggesting that remnant hole pockets survive the doping, but the holes become localized at low T in heavily doped crystals. Superconducting transition temperature (Tc) approaches zero for y = 0.14 (Co), and 0.03 (Ni), while the resistivity at the Tc onset is only weakly affected by Co doping, but it increases strongly for the Ni. These results suggest that in case of Co impurity the Tc suppression may be attributed to electron doping. On the other hand, the Ni substitution, in addition to electron doping, induces strong localization effects at small impurity contents. Using two-band conduction model we argue that the localization of electron carriers is responsible for strong superconductivity suppression by Ni impurity. Supported by EC through the FunDMS Advanced Grant of the ERC (FP7 Ideas), by the Polish NCS Grant 2011/01/B/ST3/00462, and by the French-Polish Program PICS 2012. Performed in the laboratories co-financed by NanoFun Project POIG.02.02.00-00-025/09.

Large Area Atomically Flat Surfaces via Exfoliation of Bulk Bi 2Se 3 Single Crystals

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

Melamed, Celeste L.; Ortiz, Brenden R.; Gorai, Prashun

In this paper, we present an exfoliation method that produces cm 2-area atomically flat surfaces from bulk layered single crystals, with broad applications such as for the formation of lateral heterostructures and for use as substrates for van der Waals epitaxy. Single crystals of Bi 2Se 3 were grown using the Bridgman method and examined with X-ray reciprocal space maps, Auger spectroscopy, low-energy electron diffraction, and X-ray photoelectron spectroscopy. An indium-bonding exfoliation technique was developed that produces multiple ~100 um thick atomically flat, macroscopic (>1 cm 2) slabs from each Bi 2Se 3 source crystal. Two-dimensional X-ray diffraction and reciprocalmore » space maps confirm the high crystalline quality of the exfoliated surfaces. Atomic force microscopy reveals that the exfoliated surfaces have an average root-mean-square (RMS) roughness of ~0.04 nm across 400 μm 2 scans and an average terrace width of 70 um between step edges. First-principles calculations reveal exfoliation energies of Bi 2Se 3 and a number of other layered compounds, which demonstrate relevance of our method across the field of 2D materials. While many potential applications exist, excellent lattice matching with the III-V alloy space suggests immediate potential for the use of these exfoliated layered materials as epitaxial substrates for photovoltaic development.« less

Highly Efficient LiYF4:Yb(3+), Er(3+) Upconversion Single Crystal under Solar Cell Spectrum Excitation and Photovoltaic Application.

PubMed

Chen, Xu; Xu, Wen; Song, Hongwei; Chen, Cong; Xia, Haiping; Zhu, Yongsheng; Zhou, Donglei; Cui, Shaobo; Dai, Qilin; Zhang, Jiazhong

2016-04-13

Luminescent upconversion is a promising way to harvest near-infrared (NIR) sunlight and transforms it into visible light that can be directly absorbed by active materials of solar cells and improve their power conversion efficiency (PCE). However, it is still a great challenge to effectively improve the PCE of solar cells with the assistance of upconversion. In this work, we demonstrate the application of the transparent LiYF4:Yb(3+), Er(3+) single crystal as an independent luminescent upconverter to improve the PCE of perovskite solar cells. The LiYF4:Yb(3+), Er(3+) single crystal is prepared by an improved Bridgman method, and its internal quantum efficiency approached to 5.72% under 6.2 W cm(-2) 980 nm excitation. The power-dependent upconversion luminescence indicated that under the excitation of simulated sunlight the (4)F(9/2)-(4)I(15/2) red emission originally results from the cooperation of a 1540 nm photon and a 980 nm photon. Furthermore, when the single crystal is placed in front of the perovskite solar cells, the PCE is enhanced by 7.9% under the irradiation of simulated sunlight by 7-8 solar constants. This work implies the upconverter not only can serve as proof of principle for improving PCE of solar cells but also is helpful to practical application.

Large Area Atomically Flat Surfaces via Exfoliation of Bulk Bi 2Se 3 Single Crystals

DOE PAGES

Melamed, Celeste L.; Ortiz, Brenden R.; Gorai, Prashun; ...

2017-09-12

In this paper, we present an exfoliation method that produces cm 2-area atomically flat surfaces from bulk layered single crystals, with broad applications such as for the formation of lateral heterostructures and for use as substrates for van der Waals epitaxy. Single crystals of Bi 2Se 3 were grown using the Bridgman method and examined with X-ray reciprocal space maps, Auger spectroscopy, low-energy electron diffraction, and X-ray photoelectron spectroscopy. An indium-bonding exfoliation technique was developed that produces multiple ~100 um thick atomically flat, macroscopic (>1 cm 2) slabs from each Bi 2Se 3 source crystal. Two-dimensional X-ray diffraction and reciprocalmore » space maps confirm the high crystalline quality of the exfoliated surfaces. Atomic force microscopy reveals that the exfoliated surfaces have an average root-mean-square (RMS) roughness of ~0.04 nm across 400 μm 2 scans and an average terrace width of 70 um between step edges. First-principles calculations reveal exfoliation energies of Bi 2Se 3 and a number of other layered compounds, which demonstrate relevance of our method across the field of 2D materials. While many potential applications exist, excellent lattice matching with the III-V alloy space suggests immediate potential for the use of these exfoliated layered materials as epitaxial substrates for photovoltaic development.« less

Tl2LiYCl6 (Ce3+): New Tl-based Elpasolite Scintillation Material

NASA Astrophysics Data System (ADS)

Kim, H. J.; Rooh, Gul; Park, H.; Kim, Sunghwan

2016-04-01

New single crystals of Ce-doped (1% and 10%) Tl2LiYCl6 (TLYC) were investigated under X-ray and -y-ray excitation. This material belongs to Chloro-elpasolite crystal family and was grown by the two-zone vertical Bridgman technique. X-ray-induced luminescence shows typical Ce3+ - ion emission between 350 and 530 nm peaking at 430 nm. Under 662 keV -y-rays excitation, best energy resolution of 4.8% (FWHM) was found for 1% Ce-concentration. For the same Ce-concentration, a maximum light yield of 30 500 ± 3500 ph/MeV was observed at room temperature. Under -y-ray excitation, three decay time components were observed for all Ce-doped samples. Effective Z-number and density of Tl2LiYCl6 were found to be 69 and 4.58 g/cm3, respectively. Due to highly hygroscopic nature of this compound, extra attention was devoted during handling and data taking processes. Overall, the scintillation properties confirm that this material is a promising candidate for medical imaging and radiation detection.

Electron Reconfiguration and Enhanced Phonon Activation in the Superconducting State of a FeSe0.3Te0.7 Single Crystal, as Evidenced by Mössbauer Spectroscopy

NASA Astrophysics Data System (ADS)

Greculeasa, Simona; Miu, Lucica; Badica, Petre; Nie, Jiacai; Tolea, Mugurel; Kuncser, Victor

2015-01-01

The Mössbauer spectra of a FeSe0.3Te0.7 single crystal grown by the Bridgman method were analysed across the superconducting transition by considering the interplay between the structure and electron configuration of the transition metal. The magnetically determined superconducting critical temperature is TC ˜ 14 K. The 57Fe Mössbauer spectra collected in the temperature range from 5 to 200 K mainly have an asymmetric doublet pattern, which was conveniently fitted by the full Hamiltonian method. No effective magnetic moment ascribed to the superconducting phase was observed down to 5 K. The unusual behaviour observed below ˜17 K for the chemical isomer shift and quadrupole splitting may be associated with an electron reconfiguration process intimately related to an unusual lattice distortion accompanying the superconducting transition. The decreasing trend of the total absorption spectral area and second-order Doppler shift during cooling the sample below the critical temperature, point to enhanced phonon activation in the superconducting state.

FAST TRACK COMMUNICATION: High pressure study of BaFe2As2—the role of hydrostaticity and uniaxial stress

NASA Astrophysics Data System (ADS)

Duncan, W. J.; Welzel, O. P.; Harrison, C.; Wang, X. F.; Chen, X. H.; Grosche, F. M.; Niklowitz, P. G.

2010-02-01

We investigate the evolution of the electrical resistivity of BaFe2As2 single crystals with pressure. The samples used were from the same batch, grown using a self-flux method, and showed properties that were highly reproducible. Samples were pressurized using three different pressure media: pentane-isopentane (in a piston-cylinder cell), Daphne oil (in an alumina anvil cell) and steatite (in a Bridgman cell). Each pressure medium has its own intrinsic level of hydrostaticity, which dramatically affects the phase diagram. An increasing uniaxial pressure component in this system quickly reduces the spin density wave order and favours the appearance of superconductivity, which is similar to what is seen in SrFe2As2.

Growth and luminescent properties of Ce and Eu doped Cesium Hafnium Iodide single crystalline scintillators

NASA Astrophysics Data System (ADS)

Kodama, Shohei; Kurosawa, Shunsuke; Yamaji, Akihiro; Pejchal, Jan; Král, Robert; Ohashi, Yuji; Kamada, Kei; Yokota, Yuui; Nikl, Martin; Yoshikawa, Akira

2018-06-01

In order to obtain new scintillators with high light output and high effective atomic number (Zeff), we performed anion-substitution for Cs2HfCl6 (CHC) scintillator, and then, we succeeded in growing Cs2HfI6 (CHI) single crystalline scintillator. It had Zeff of 58, which is the same as that of CHC, and had high light output of ∼70,000 photons/MeV with 700 nm emission. However, its scintillation decay time of ∼2.5 μs was slow for practical use as gamma-ray monitor. In this study, we performed Ce3+/Eu2+ doping to Hf4+ site to improve decay time of CHI, introducing the fast 5d-4f luminescence. Ce:CHI and Eu:CHI single crystals were finally obtained by the vertical Bridgman-Stockbarger method. The luminescence spectra of the Ce:CHI and Eu:CHI were very similar to that of the non-doped CHI, which would mean that no 5d-4f luminescence of Ce3+/Eu2+ was observed. The measured light output and decay time of Ce:CHI were ∼48,000 photon/MeV and 2.3 ± 0.1 μs, respectively. As for Eu:CHI, light output and decay time were ∼69,000 photon/MeV and 2.8 ± 0.1 μs, respectively.

Electrical conductivity and dielectric properties of TlInS2 single crystals

NASA Astrophysics Data System (ADS)

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

2011-07-01

TlInS2 single crystals were grown by using Bridgman-Stockbauer technique. Measurements of DC conductivity were carried out in parallel (σ//) and perpendicular (σ⊥) directions to the c-axis over a temperature range from 303 to 463 K. The anisotropic behaviour of the electrical conductivity was also detected. AC conductivity and dielectric measurements were studied as a function of both frequency (102-106 Hz) and temperature (297-375 K). The frequency dependence of the AC conductivity revealed that σac(ω) obeys the universal law: σac(ω) = Aωs. The mechanism of the ac charge transport across the layers of TlInS2 single crystals was referred to the hopping over localized states near the Fermi level in the frequency range >3.5 × 103 Hz. The temperature dependence of σac(ω) for TlInS2 showed that σac is thermally activated process. Both of ɛ1 and ɛ2 decrease by increasing frequency and increase by increasing temperature. Some parameters were calculated as: the density of localized states near the Fermi level NF = 1.5 × 1020 eV-1 cm-3, the average time of charge carrier hoping between localized states τ = 3.79 μs and the average hopping distance R = 6.07 nm.

Tuning the structure of CsCaI3:Eu via substitution of bromine for iodine

NASA Astrophysics Data System (ADS)

Loyd, M.; Lindsey, A.; Stand, L.; Zhuravleva, M.; Melcher, C. L.; Koschan, M.

2017-06-01

CsCaI3:Eu is a promising scintillator material that can be grown from the melt, but undergoes a tetragonal to orthorhombic phase transition upon cooling at 255 °C, causing twinning and cloudiness. The purpose of this work is to suppress this solid to solid phase transition in the CsCaI3:Eu scintillator, which has a light yield of ∼40000 ph/MeV and energy resolution at 662 keV of ∼4%, by halide replacement to form the compound CsCaBrxI3-x. Crystals 8 cm3 in volume were grown using the vertical Bridgman method with varying bromine content from x = 0.2 to x = 1, resulting in improved transparency for crystals with bromine content x > 0.6. Powder X-ray diffraction data coupled with differential scanning calorimetry and radioluminescence measurements were used to investigate structural modifications, melting point dependence and spectral emission dependence on the bromine/iodine ratio. Partial replacement of iodine by bromine improves optical quality and scintillation properties by stabilizing the structure, rendering it useful for isotope identification for national security applications. The composition CsCaBr0.8I2.2:Eu was determined to be the best combination of improved structure and performance, and larger 22 and 38 mm Ø crystals were grown for further evaluation. Large size slabs of these crystals showed good crystal quality and improved performance over CsCaI3Eu with 8.4% and 9.5% energy resolution at 662 keV, respectively.

High pressure as a probe of the solid state

NASA Astrophysics Data System (ADS)

Ruoff, Arthur L.

1994-07-01

It is a great pleasure and honor to receive the Percy Williams Bridgman Award. Henry Eyring, my Ph.D. advisor, instilled in me a desire to unravel the secrets of nature in the chemical and physical world. He continued what my mother had begun. From my father I learned the virtue and satisfaction of hard work. In reading Percy Bridgman's The Physics of High Pressure [1] after I came to Cornell, I became intrigued by the high-pressure variable, so I owe much to him. I received valuable assistance and encouragement from George Kennedy and Harry Drickamer (the first winner of the Bridgman Award) and later from Alvin Van Valkenburg (a co-inventor with three others of the diamond anvil cell). Most importantly, I received encouragement from my wife, Enid Seaton Ruoff, to carry out what is sometimes the arduous pursuit of science—a pursuit that involves long working hours—and I want especially to thank her.

Single crystals of the fluorite nonstoichiometric phase Eu{0.916/2+}Eu{0.084/3+}F2.084 (conductivity, transmission, and hardness)

NASA Astrophysics Data System (ADS)

Sobolev, B. P.; Turkina, T. M.; Sorokin, N. I.; Karimov, D. N.; Komar'kova, O. N.; Sulyanova, E. A.

2010-07-01

The nonstoichiometric phase EuF2+ x has been obtained via the partial reduction of EuF3 by elementary Si at 900-1100°C. Eu{0.916/2+}Eu{0.084/3+}F2.084 (EuF2.084) single crystals have been grown from melt by the Bridgman method in a fluorinating atmosphere. These crystals belong to the CaF2 structure type (sp. gr. Fm bar 3 m) with the cubic lattice parameter a = 5.8287(2) Å, are transparent in the spectral range of 0.5-11.3 μm, and have microhardness H μ = 3.12 ± 0.13 GPa and ionic conductivity σ = 1.4 × 10-5 S/cm at 400°C with the ion transport activation energy E a = 1.10 ± 0.05 eV. The physicochemical characteristics of the fluorite phases in the EuF2 - EuF3 systems are similar to those of the phases in the SrF2 - EuF3 and SrF2 - GdF3 systems due to the similar lattice parameters of the EuF2 and SrF2 components. Europium difluoride supplements the list of fluorite components MF2 ( M = Ca, Sr, Ba, Cd, Pb), which are crystal matrices for nonstoichiometric (nanostructured) fluoride materials M 1 - x R x F2 + x ( R are rare earth elements).

Protein crystal growth; Proceedings of the First International Conference, Stanford University, CA, August 14-16, 1985

NASA Technical Reports Server (NTRS)

Feigelson, R. S. (Editor)

1986-01-01

Papers are presented on mechanisms of nucleation and growth of protein crystals, the role of purification in the crystallization of proteins and nucleic acids, and the effect of chemical impurities in polyethylene glycol on macromolecular crystallization. Also considered are growth kinetics of tetragonal lysozyme crystals, thermodynamic and kinetic considerations for crystal growth of complex molecules from solution, protein single-crystal growth under microgravity, and growth of organic crystals in a microgravity environment. Papers are also presented on preliminary investigations of protein crystal growth using the Space Shuttle, convective diffusion in protein crystal growth, and the growth and characterization of membrane protein crystals.

Natural convection in the Hale-Shaw cell of horizontal Bridgman solidification

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

Lu, Y.; Liu, J.; Zhou, Y.

1995-08-01

The numerical simulation of natural convection in the Hale-Shaw cell during horizontal Bridgman solidification reveals that the convection is present even for the very thin cell. The effects of the horizontal temperature gradient, G, thickness of the cell, H, temperature difference between the top and bottom of the cell, and other parameters have been studied. These findings have been confirmed by experiments through direct observation and measurement of convection in the cell containing succinonitrile transparent model alloy.

Polarization-selective three-photon absorption and subsequent photoluminescence in CsPbBr3 single crystal at room temperature

NASA Astrophysics Data System (ADS)

Clark, D. J.; Stoumpos, C. C.; Saouma, F. O.; Kanatzidis, M. G.; Jang, J. I.

2016-05-01

We report on highly polarization-selective three-photon absorption (3PA) in a Bridgman-grown single crystal of CsPbBr3 oriented along the (112) direction, which is an inorganic counterpart to emerging organic-inorganic hybrid halide perovskites for solar-cell and optoelectronic applications. The crystal exhibits strong photoluminescence (PL) at room temperature as a direct consequence of 3PA of fundamental radiation. Interestingly, 3PA disappears when the input polarization is parallel to the (-110 ) direction. This 3PA effect is strongest when orthogonal to (-110 ) and the corresponding 3PA coefficient was measured to be γ =0.14 ±0.03 cm3/GW2 under picosecond-pulse excitation at the fundamental wavelength of λ =1200 nm. The laser-induced damage threshold was also determined to be about 20 GW/cm2 at the same wavelength. Based on relative PL intensities upon λ tuning over the entire 3PA range (1100 -1700 nm), we determined the nonlinear optical dispersion of the 3PA coefficient for CsPbBr3, which is consistent with a theoretical prediction. Experimentally observed significant polarization dependence of γ was explained by relevant selection rules. The perovskite is potentially important for nonlinear optical applications owing to its highly efficient 3PA-induced PL response with a sharp on/off ratio by active polarization control.

Cu2I2Se6: A Metal-Inorganic Framework Wide-Bandgap Semiconductor for Photon Detection at Room Temperature.

PubMed

Lin, Wenwen; Stoumpos, Constantinos C; Kontsevoi, Oleg Y; Liu, Zhifu; He, Yihui; Das, Sanjib; Xu, Yadong; McCall, Kyle M; Wessels, Bruce W; Kanatzidis, Mercouri G

2018-02-07

Cu 2 I 2 Se 6 is a new wide-bandgap semiconductor with high stability and great potential toward hard radiation and photon detection. Cu 2 I 2 Se 6 crystallizes in the rhombohedral R3̅m space group with a density of d = 5.287 g·cm -3 and a wide bandgap E g of 1.95 eV. First-principles electronic band structure calculations at the density functional theory level indicate an indirect bandgap and a low electron effective mass m e * of 0.32. The congruently melting compound was grown in centimeter-size Cu 2 I 2 Se 6 single crystals using a vertical Bridgman method. A high electric resistivity of ∼10 12 Ω·cm is readily achieved, and detectors made of Cu 2 I 2 Se 6 single crystals demonstrate high photosensitivity to Ag Kα X-rays (22.4 keV) and show spectroscopic performance with energy resolutions under 241 Am α-particles (5.5 MeV) radiation. The electron mobility is measured by a time-of-flight technique to be ∼46 cm 2 ·V -1 ·s -1 . This value is comparable to that of one of the leading γ-ray detector materials, TlBr, and is a factor of 30 higher than mobility values obtained for amorphous Se for X-ray detection.

High pressure as a probe of the solid state

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

Ruoff, A.L.

1994-07-10

It is a great pleasure and honor to receive the Percy Williams Bridgman Award. Henry Eyring, my Ph.D. advisor, instilled in me a desire to unravel the secrets of nature in the chemical and physical world. He continued what my mother had begun. From my father I learned the virtue and satisfaction of hard work. In reading Percy Bridgman's [ital The] [ital Physics] [ital of] [ital High] [ital Pressure] [1] after I came to Cornell, I became intrigued by the high-pressure variable, so I owe much to him. I received valuable assistance and encouragement from George Kennedy and Harry Drickamermore » (the first winner of the Bridgman Award) and later from Alvin Van Valkenburg (a co-inventor with three others of the diamond anvil cell). Most importantly, I received encouragement from my wife, Enid Seaton Ruoff, to carry out what is sometimes the arduous pursuit of science---a pursuit that involves long working hours---and I want especially to thank her. [copyright] 1994 American Institute of Physics« less

GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

DTIC Science & Technology

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

Electronic structure and optical properties of Cs2HgI4: Experimental study and band-structure DFT calculations

NASA Astrophysics Data System (ADS)

Lavrentyev, A. A.; Gabrelian, B. V.; Vu, V. T.; Shkumat, P. N.; Myronchuk, G. L.; Khvyshchun, M.; Fedorchuk, A. O.; Parasyuk, O. V.; Khyzhun, O. Y.

2015-04-01

High-quality single crystal of cesium mercury tetraiodide, Cs2HgI4, has been synthesized by the vertical Bridgman-Stockbarger method and its crystal structure has been refined. In addition, electronic structure and optical properties of Cs2HgI4 have been studied. For the crystal under study, X-ray photoelectron core-level and valence-band spectra for pristine and Ar+-ion irradiated surfaces have been measured. The present X-ray photoelectron spectroscopy (XPS) results indicate that the Cs2HgI4 single crystal surface is very sensitive with respect to Ar+ ion-irradiation. In particular, Ar+ bombardment of the single crystal surface alters the elemental stoichiometry of the Cs2HgI4 surface. To elucidate peculiarities of the energy distribution of the electronic states within the valence-band and conduction-band regions of the Cs2HgI4 compound, we have performed first-principles band-structure calculations based on density functional theory (DFT) as incorporated in the WIEN2k package. Total and partial densities of states for Cs2HgI4 have been calculated. The DFT calculations reveal that the I p states make the major contributions in the upper portion of the valence band, while the Hg d, Cs p and I s states are the dominant contributors in its lower portion. Temperature dependence of the light absorption coefficient and specific electrical conductivity has been explored for Cs2HgI4 in the temperature range of 77-300 K. Main optical characteristics of the Cs2HgI4 compound have been elucidated by the first-principles calculations.

On the origin of size-dependent and size-independent crystal growth: Influence of advection and diffusion

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

2003-01-01

Crystal growth experiments were conducted using potassium alum and calcite crystals in aqueous solution under both non-stirred and stirred conditions to elucidate the mechanism for size-dependent (proportionate) and size-independent (constant) crystal growth. Growth by these two laws can be distinguished from each other because the relative size difference among crystals is maintained during proportionate growth, leading to a constant crystal size variance (??2) for a crystal size distribution (CSD) as the mean size increases. The absolute size difference among crystals is maintained during constant growth, resulting in a decrease in size variance. Results of these experiments show that for centimeter-sized alum crystals, proportionate growth occurs in stirred systems, whereas constant growth occurs in non-stirred systems. Accordingly, the mechanism for proportionate growth is hypothesized to be related to the supply of reactants to the crystal surface by advection, whereas constant growth is related to supply by diffusion. Paradoxically, micrometer-sized calcite crystals showed proportionate growth both in stirred and in non-stirred systems. Such growth presumably results from the effects of convection and Brownian motion, which promote an advective environment and hence proportionate growth for minute crystals in non-stirred systems, thereby indicating the importance of solution velocity relative to crystal size. Calcite crystals grown in gels, where fluid motion was minimized, showed evidence for constant, diffusion-controlled growth. Additional investigations of CSDs of naturally occurring crystals indicate that proportionate growth is by far the most common growth law, thereby suggesting that advection, rather than diffusion, is the dominant process for supplying reactants to crystal surfaces.

GaSb and Ga1-xInxSb Thermophotovoltaic Cells using Diffused Junction Technology in Bulk Substrates

NASA Astrophysics Data System (ADS)

Dutta, P. S.; Borrego, J. M.; Ehsani, H.; Rajagopalan, G.; Bhat, I. B.; Gutmann, R. J.; Nichols, G.; Baldasaro, P. F.

2003-01-01

This paper presents results of experimental and theoretical research on antimonide- based thermophotovoltaic (TPV) materials and cells. The topics discussed include: growth of large diameter ternary GaInSb bulk crystals, substrate preparation, diffused junction processes, cell fabrication and characterization, and, cell modeling. Ternary GaInSb boules up to 2 inches in diameter have been grown using the vertical Bridgman technique with a novel self solute feeding technique. A single step diffusion process followed by precise etching of the diffused layer has been developed to obtain a diffusion profile appropriate for high efficiency, p-n junction GaSb and GaInSb thermophotovoltaic cells. The optimum junction depth to obtain the highest quantum efficiency and open circuit voltage has been identified based on diffusion lengths (or minority carrier lifetimes), carrier mobility and experimental diffused impurity profiles. Theoretical assessment of the performance of ternary (GaInSb) and binary (GaSb) cells fabricated by Zn diffusion in bulk substrates has been performed using PC-1D one-dimensional computer simulations. Several factors affecting the cell performances such as the effects of emitter doping profile, emitter thickness and recombination mechanisms (Auger, radiative and Shockley-Read-Hall), the advantages of surface passivation and the impact of dark current due to the metallic grid will be discussed. The conditions needed for diffused junction cells on ternary and binary substrates to achieve similar performance to the epitaxially grown lattice- matched quaternary cells are identified.

Process modelling for materials preparation experiments

NASA Technical Reports Server (NTRS)

Rosenberger, Franz; Alexander, J. Iwan D.

1994-01-01

The main goals of the research under this grant consist of the development of mathematical tools and measurement techniques for transport properties necessary for high fidelity modelling of crystal growth from the melt and solution. Of the tasks described in detail in the original proposal, two remain to be worked on: development of a spectral code for moving boundary problems, and development of an expedient diffusivity measurement technique for concentrated and supersaturated solutions. We have focused on developing a code to solve for interface shape, heat and species transport during directional solidification. The work involved the computation of heat, mass and momentum transfer during Bridgman-Stockbarger solidification of compound semiconductors. Domain decomposition techniques and preconditioning methods were used in conjunction with Chebyshev spectral methods to accelerate convergence while retaining the high-order spectral accuracy. During the report period we have further improved our experimental setup. These improvements include: temperature control of the measurement cell to 0.1 C between 10 and 60 C; enclosure of the optical measurement path outside the ZYGO interferometer in a metal housing that is temperature controlled to the same temperature setting as the measurement cell; simultaneous dispensing and partial removal of the lower concentration (lighter) solution above the higher concentration (heavier) solution through independently motor-driven syringes; three-fold increase in data resolution by orientation of the interferometer with respect to diffusion direction; and increase of the optical path length in the solution cell to 12 mm.

Lamellar boundary alignment of DS-processed TiAl-W alloys by a solidification procedure

NASA Astrophysics Data System (ADS)

Jung, In-Soo; Oh, Myung-Hoon; Park, No-Jin; Kumar, K. Sharvan; Wee, Dang-Moon

2007-12-01

In this study, a β solidification procedure was used to align the lamellae in a Ti-47Al-2W (at.%) alloy parallel to the growth direction. The Bridgman technique and the floating zone process were used for directional solidification. The mechanical properties of the directionally solidified alloy were evaluated in tension at room temperature and at 800°C. At a growth rate of 30 mm/h (with the floating zone approach), the lamellae were well aligned parallel to the growth direction. The aligned lamellae yielded excellent room temperature tensile ductility. The tensile yield strength at 800°C was similar to that at room temperature. The orientation of the γ lamellar laths in the directionally solidified ingots, which were manufactured by means of a floating zone process, was identified with the aid of electron backscattered diffraction analysis. On the basis of this analysis, the preferred growth direction of the bcc-β dendrites that formed at high temperatures close to the melting point was inferred to be [001]β at a growth rate of 30 mm/h and [111]β at a growth rate of 90 mm/h.

Investigating new activators for small-bandgap LaX3 (X = Br, I) scintillators

NASA Astrophysics Data System (ADS)

Rutstrom, Daniel; Collette, Robyn; Stand, Luis; Loyd, Matthew; Wu, Yuntao; Koschan, Merry; Melcher, Charles L.; Zhuravleva, Mariya

2018-02-01

Luminescence and scintillation properties of Bi3+, Sb3+, and Eu2+-doped LaI3 and LaBr3 were explored. Out of the three dopants investigated, Eu2+ was the most promising new activator for small-bandgap LaX3 (X = Br, I) and was further studied in the mixed-halide LaBr3-xIx. Crystals were grown from the melt using the vertical Bridgman method. LaBr3:Eu2+ 0.5% (mol) had the most favorable scintillation properties with a light output of 43,000 ph/MeV and 6% energy resolution at 662 keV. Performance of LaBr3-xIx:Eu2+ worsened for most samples as iodide concentration was increased. Room-temperature scintillation of LaI3:Eu2+ 0.1% and 0.5% was observed and is the first case of room-temperature emission reported for doped LaI3.

Control of interface shape during high melting sesquioxide crystal growth by HEM technique

NASA Astrophysics Data System (ADS)

Hu, Kaiwei; Zheng, Lili; Zhang, Hui

2018-02-01

During crystal growth in heat exchanger method (HEM) system, the shape of the growth interface changes with the proceeding of the growth process, which limits the crystal size and reduces the quality of the crystal. In this paper, a modified HEM system is proposed to control the interface shape for growth of sesquioxide crystals. Numerical simulation is performed to predict heat transfer, melt flow and interface shape during growth of high melting sesquioxide crystals by the heat exchanger method. The results show that a flat or slightly convex interface shape is beneficial to reduce the solute pileup in front of the melt/crystal interface and decrease the radial temperature gradient inside the crystal during growth of sesquioxide crystals. The interface shape can be controlled by adjusting the gap size d and lower resistance heater power during growth. The growth rate and the melt/crystal interface position can be obtained by two measured temperatures.

Surrogate Seeds For Growth Of Crystals

NASA Technical Reports Server (NTRS)

Shlichta, Paul J.

1989-01-01

Larger crystals of higher quality grown. Alternative method for starting growth of crystal involves use of seed crystal of different material instead of same material as solution. Intended for growing single-crystal proteins for experiments but applicable in general to growth of crystals from solutions and to growth of semiconductor or other crystals from melts.

Detailed Studies of Pixelated CZT Detectors Grown with the Modified Horizontal Bridgman Method

NASA Technical Reports Server (NTRS)

Jung, I.; Krawczynski, H.; Burger, A.; Guo, M.; Groza, M.

2007-01-01

The detector material Cadmium Zinc Telluride (CZT) achieves excellent spatial resolution and good energy resolution over a broad energy range, several keV up to some MeV. Presently, there are two main methods to grow CZT crystals, the Modified High-Pressure Bridgman (MHB) and the High-Pressure Bridgman (HPB) process. The study presented in this paper is based on MHB CZT substrates from the company Orbotech Medical Solutions Ltd. [Orbotech Medical Solutions Ltd., 10 Plaut St., Park Rabin, P.O. Box 2489, Rehovot, Israel, 76124]. Former studies have shown that high-work-function materials on the cathode side reduce the leakage current and, therefore, improve the energy resolution at lower energies. None of the studies have emphasized on the anode contact material. Therefore, we present in this paper the result of a detailed study in which for the first time the cathode material was kept constant and the anode material was varied. We used four different anode materials: Indium, Titanium, Chromium and Gold, metals with work-functions between 4.1 eV and 5.1 eV. The detector size was 2.0 x 2.0 x 0.5 cu cm with 8 x 8 pixels and a pitch of 2.46 mm. The best performance was achieved with the low-work-function materials Indium and Titanium with energy resolutions of 2.0 keV (at 59 keV) and 1.9 keV (at 122 keV) for Titanium and 2.1 keV (at 59 keV) and 2.9 keV (at 122 keV) for Indium. Taking into account the large pixel pitch of 2.46 mm, these resolutions are very competitive in comparison to those achieved with detectors made of material produced with the more expensive conventional HPB method. We present a detailed comparison of our detector response with 3D simulations. The latter comparisons allow us to determine the mobility-lifetime-products (mu tau-products) for electrons and holes. Finally, we evaluated the temperature dependency of the detector performance and ls-products. For many applications temperature dependence is important, therefore, we extended the scope of our study to temperatures as low as -30 C. There are two important results. The breakdown voltage increases with decreasing temperature, and electron mobility-lifetime-product decreases by about 30% over a range from 20 C to -30 C. The latter effect causes the energy resolution to deteriorate, but the concomitantly increasing breakdown voltage makes it possible to increase the applied bias voltage and restore the full performance

Ternary eutectic growth of nanostructured thermoelectric Ag-Pb-Te materials

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

Wu, Hsin-jay; Chen, Sinn-wen; Foo, Wei-jian

2012-07-09

Nanostructured Ag-Pb-Te thermoelectric materials were fabricated by unidirectionally solidifying the ternary Ag-Pb-Te eutectic and near-eutectic alloys using the Bridgeman method. Specially, the Bridgman-grown eutectic alloy exhibited a partially aligned lamellar microstructure, which consisted of Ag{sub 5}Te{sub 3} and Te phases, with additional 200-600 nm size particles of PbTe. The self-assembled interfaces altered the thermal and electronic transport properties in the bulk Ag-Pb-Te eutectic alloy. Presumably due to phonon scattering from the nanoscale microstructure, a low thermal conductivity ({kappa} = 0.3 W/mK) was achieved of the eutectic alloy, leading to a zT peak of 0.41 at 400 K.

Thermoluminescence dosimetric characteristics on cubic fluoroperovskite single crystal (KMgF3:Eu2+, Ce3+)

NASA Astrophysics Data System (ADS)

Joseph Daniel, D.; Madhusoodanan, U.; Annalakshmi, O.; Jose, M. T.; Ramasamy, P.

2015-07-01

This paper describes investigation of thermoluminescence radiation dosimetry characteristics of Eu2+ doped Potassium Magnesium Fluoride (KMgF3) single crystal co-doped with Ce3+ ions. The perovskite-like KMgF3 polycrystalline compounds were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of KMgF3 have been grown from melt by using a vertical Bridgman-Stockbarger method. Thermoluminescence (TL) characteristics of KMgF3 samples doped with Eu2+ and Ce3+ have been studied after β-ray irradiation at room temperature. Order of kinetics (b), activation energy (E), and frequency factor (s) were determined by Chen's method and variable heating rate method. Results show that the TL glow peak of the KMgF3 samples obeys second-order kinetics. Analysis of the main dosimetric peak by using the methods mentioned above revealed that activation energy (E) is about 1.2 eV and the frequency factor (s) is in the range 1010-1011 s-1. The TL glow curve structure of the sample remained stable for higher doses of 90Sr/90Y beta source and it shows linearity up to 180 Gy. The time dependent fading behavior of the TL characteristics has also been investigated and is found to be quite stable over long time duration. The characteristic Eu2+ emissions are observed in the TL emission spectra.

Unsteady-state transfer of impurities during crystal growth of sucrose in sugarcane solutions

NASA Astrophysics Data System (ADS)

Martins, P. M.; Ferreira, A.; Polanco, S.; Rocha, F.; Damas, A. M.; Rein, P.

2009-07-01

In this work, we present growth rate data of sucrose crystals in the presence of impurities that can be used by both sugar technologists and crystal growth scientists. Growth rate curves measured in a pilot-scale evaporative crystallizer suggest a period of slow growth that follows the seeding of crystals into supersaturated technical solutions. The observed trend was enhanced by adding typical sugarcane impurities such as starch, fructose or dextran to the industrial syrups. Maximum growth rates of sucrose resulted at intermediate rather than high supersaturation levels in the presence of the additives. The effects of the additives on the sucrose solubility and sucrose mass transfer in solution were taken into account to explain the observed crystal growth kinetics. A novel mechanism was identified of unsteady-state adsorption of impurities at the crystal surface and their gradual replacement by the crystallizing solute towards the equilibrium occupation of the active sites for growth. Specifically designed crystallization experiments at controlled supersaturation confirmed this mechanism by showing increasing crystal growth rates with time until reaching a steady-state value for a given supersaturation level and impurity content.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

An Apparatus for Growth of Small Crystals From Solutions.

ERIC Educational Resources Information Center

Mitrovic, Mico M.

1995-01-01

Describes an apparatus for crystal growth that was designed to study growth kinetics of small crystals from solutions and to obtain crystals of various substances. Describes the use of the apparatus in laboratory practical experiments in the field of crystal growth physics within the course "Solid State Physics". (JRH)

Solution Growth and Characterization of Single Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Currie, J. R.; Penn, B. G.; Batra, A. K.; Lal, R. B.

2007-01-01

Crystal growth has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high-technology devices, and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this Technical Memorandum (TM) an attempt is made to give the fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, the authors proposed a new cooled-sting technique to grow crystals in space. The authors experience from conducting two Space Shuttle solution crystal growth experiments are also detailed in this TM and the complexity of solution growth experiments to grow crystals in space are also discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that shares basic principles of the solution growth technique is given, along with some flight hardware information for growth in microgravity.

Growth and Characteristics of Bulk Single Crystals Grown from Solution on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Batra, A. K.; Lal, R. B.; Penn, Benjamin G.; Frazier, Donald O.

2011-01-01

The growth of crystals has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high technology devices and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this chapter an attempt is made to give some fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, authors had proposed a new cooled sting technique to grow crystals in space. Authors? experiences of conducting two space shuttle experiments relating to solution crystal growth are also detailed in this work. The complexity of these solution growth experiments to grow crystals in space are discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that also shares basic principles of solution growth technique is given along with some flight hardware information for its growth in microgravity.

Microstructural development and segregation effects in directionally solidified nickel-based superalloy PWA 1484

NASA Astrophysics Data System (ADS)

Li, Lichun

2002-09-01

These studies were performed to investigate the effects of thermal gradient (G) and growth velocity (V) on the microstructure development and solidification behavior of directionally solidified nickel-based superalloy PWA 1484. Directional solidification (DS) experiments were conducted using a Bridgman crystal growth facility. The solidification velocity ranged from 0.00005 to 0.01 cm/sec and thermal gradients ranged from 12 to 108°C/cm. The as-cast microstructures of DS samples were characterized by using conventional metallography; chemical composition and segregation of directionally solidified samples were analyzed with energy dispersive spectroscopy in SEM. A range of aligned solidification microstructures is exhibited by the alloy when examined as-cast at room temperature: dendrites, flanged cells, cells. The microstructure transitions from cellular to dendritic as the growth velocity increases. The experimental data for PWA1484 exhibits excellent agreement with the well-known exponential equation (lambda1 ∝ G -1/2V-1/4). However, the constant of proportionality is different depending upon the solidification microstructure: (1) dendritic growth with secondary arms leads to a marked dependence of lambda1 on G-1/2 V-1/4; (2) flanged cellular growth with no secondary arms leads to much lower dependence of lambda 1 on G-1/2V -1/4. The primary dendritic arm spacing results were also compared to recent theoretical models. The model of Hunt and Lu and the model of Ma and Sahm provided excellent agreement at medium to high thermal gradients and a wide range of solidification velocities. The anomalous behavior of lambda 1 with high growth velocity V at low G is analyzed based on the samples' microstructures. Off-axis heat flows were shown to cause radial non-uniformity in the dendrite arm spacing data for low thermal gradients and large withdrawal velocities. Various precipitates including gamma', (gamma ' + gamma) eutectic pool or divorced eutectic gamma ', and metal carbides were characterized. Processing conditions (growth velocity V and thermal gradient G) exert significant influence on both morphology and size of precipitates present. Freckle defects were observed on the surface of nickel-based superalloy MM247 cylindrical samples but not on the surface of cylindrical PWA 1484 samples. The Rayleigh number (Ra) that represents liquid instability at the interface was evaluated for MM247 and PWA 1484 in terms of a recently proposed theoretical equation. The effects of segregation, sloped solid/liquid interface and the morphology of dendritic/cellular trunks on the mushy zone convective flow and freckle formation are also discussed.

Modeling Czochralski growth of oxide crystals for piezoelectric and optical applications

NASA Astrophysics Data System (ADS)

Stelian, C.; Duffar, T.

2018-05-01

Numerical modeling is applied to investigate the impact of crystal and crucible rotation on the flow pattern and crystal-melt interface shape in Czochralski growth of oxide semi-transparent crystals used for piezoelectric and optical applications. Two cases are simulated in the present work: the growth of piezoelectric langatate (LGT) crystals of 3 cm in diameter in an inductive furnace, and the growth of sapphire crystals of 10 cm in diameter in a resistive configuration. The numerical results indicate that the interface shape depends essentially on the internal radiative heat exchanges in the semi-transparent crystals. Computations performed by applying crystal/crucible rotation show that the interface can be flattened during LGT growth, while flat-interface growth of large diameter sapphire crystals may not be possible.

Application of enthalpy model for floating zone silicon crystal growth

NASA Astrophysics Data System (ADS)

Krauze, A.; Bergfelds, K.; Virbulis, J.

2017-09-01

A 2D simplified crystal growth model based on the enthalpy method and coupled with a low-frequency harmonic electromagnetic model is developed to simulate the silicon crystal growth near the external triple point (ETP) and crystal melting on the open melting front of a polycrystalline feed rod in FZ crystal growth systems. Simulations of the crystal growth near the ETP show significant influence of the inhomogeneities of the EM power distribution on the crystal growth rate for a 4 in floating zone (FZ) system. The generated growth rate fluctuations are shown to be larger in the system with higher crystal pull rate. Simulations of crystal melting on the open melting front of the polycrystalline rod show the development of melt-filled grooves at the open melting front surface. The distance between the grooves is shown to grow with the increase of the skin-layer depth in the solid material.

Protein crystal growth in microgravity

NASA Technical Reports Server (NTRS)

Rosenblum, William M.; Delucas, Lawrence J.; Wilson, William W.

1989-01-01

Major advances have been made in several of the experimental aspects of protein crystallography, leaving protein crystallization as one of the few remaining bottlenecks. As a result, it has become important that the science of protein crystal growth is better understood and that improved methods for protein crystallization are developed. Preliminary experiments with both small molecules and proteins indicate that microgravity may beneficially affect crystal growth. For this reason, a series of protein crystal growth experiments using the Space Shuttle was initiated. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth. Various optical techniques are being utilized to monitor the crystal growth process from the incipient or nucleation stage and throughout the growth phase. The eventual goal of these studies is to develop a system which utilizes optical monitoring for dynamic control of the crystallization process.

Protein crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1988-01-01

Protein crystal growth is a major experimental problem and is the bottleneck in widespread applications of protein crystallography. Research efforts now being pursued and sponsored by NASA are making fundamental contributions to the understanding of the science of protein crystal growth. Microgravity environments offer the possibility of performing new types of experiments that may produce a better understanding of protein crystal growth processes and may permit growth environments that are more favorable for obtaining high quality protein crystals. A series of protein crystal growth experiments using the space shuttle was initiated. The first phase of these experiments was focused on the development of micro-methods for protein crystal growth by vapor diffusion techniques, using a space version of the hanging drop method. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth.

Kinetic Roughening Transition and Energetics of Tetragonal Lysozyme Crystal Growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2004-01-01

Interpretation of lysozyme crystal growth rates using well-established physical theories enabled the discovery of a phenomenon possibly indicative of kinetic roughening. For example, lysozyme crystals grown above a critical supersaturation sigma, (where supersaturation sigma = ln c/c(sub eq), c = the protein concentration and c(sub eq) = the solubility concentration) exhibit microscopically rough surfaces due to the continuous addition of growth units anywhere on the surface of a crystal. The rate of crystal growth, V(sub c), for the continuous growth process is determined by the continuous flux of macromolecules onto a unit area of the crystal surface, a, from a distance, xi, per unit time due to diffusion, and a probability of attachment onto the crystal surface, expressed. Based upon models applied, the energetics of lysozyme crystal growth was determined. The magnitudes of the energy barriers of crystal growth for both the (110) and (101) faces of tetragonal lysozyme crystals are compared. Finally, evidence supportive of the kinetic roughening hypothesis is presented.

Crystal growth in fused solvent systems

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Noone, M. J.; Spear, K. E.; White, W. B.; Henry, E. C.

1973-01-01

Research is reported on the growth of electronic ceramic single crystals from solution for the future growth of crystals in a microgravity environment. Work included growth from fused or glass solvents and aqueous solutions. Topics discussed include: crystal identification and selection; aqueous solution growth of triglycine sulphate (TGS); and characterization of TGS.

Phenytoin crystal growth rates in the presence of phosphate and chloride ions

NASA Astrophysics Data System (ADS)

Zipp, G. L.; Rodríguez-Hornedo, N.

1992-09-01

Phenytoin crystal growth kinetics have been measured as a function of supersaturation in pH 2.2 phosphoric acid and pH 2.2 hydrochloric acid solutions. Two different methods were used for the kinetic analysis. The first involved a zone-sensing device which provided an analysis of the distribution of crystals in a batch crystallizer. Crystal growth rates were calculated from the increase in the size of the distribution with time. In the second method, growth rates were evaluated from the change in size with time of individual crystals observed under an inverted microscope. The results from each method compare favorably. The use of both techniques provides an excellent opportunity to exploit the strengths of each: an average growth rate from a population of crystals from batch crystallization and insight into the effect of growth on the morphology of the crystals from the individual crystal measurements.

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Pusey, M.; Snell, E.; Judge, R.; Chayen, N.; Boggon, T.

2000-01-01

The molecular structure of biological macromolecules is important in understanding how these molecules work and has direct application to rational drug design for new medicines and for the improvement and development of industrial enzymes. In order to obtain the molecular structure, large, well formed, single macromolecule crystals are required. The growth of macromolecule crystals is a difficult task and is often hampered on the ground by fluid flows that result from the interaction of gravity with the crystal growth process. One such effect is the bulk movement of the crystal through the fluid due to sedimentation. A second is buoyancy driven convection close to the crystal surface. On the ground the crystallization process itself induces both of these flows. Buoyancy driven convection results from density differences between the bulk solution and fluid close to the crystal surface which has been depleted of macromolecules due to crystal growth. Schlieren photograph of a growing lysozyme crystal illustrating a 'growth plume' resulting from buoyancy driven convection. Both sedimentation and buoyancy driven convection have a negative effect on crystal growth and microgravity is seen as a way to both greatly reduce sedimentation and provide greater stability for 'depletion zones' around growing crystals. Some current crystal growth hardware however such as those based on a vapor diffusion techniques, may also be introducing unwanted Marangoni convection which becomes more pronounced in microgravity. Negative effects of g-jitter on crystal growth have also been observed. To study the magnitude of fluid flows around growing crystals we have attached a number of different fluorescent probes to lysozyme molecules. At low concentrations, less than 40% of the total protein, the probes do not appear to effect the crystal growth process. By using these probes we expect to determine not only the effect of induced flows due to crystal growth hardware design but also hope to optimize crystallization hardware so that destructive flows are minimized both on the ground and in microgravity.

Contact Angles and Surface Tension of Germanium-Silicon Melts

NASA Technical Reports Server (NTRS)

Croell, A.; Kaiser, N.; Cobb, S.; Szofran, F. R.; Volz, M.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Precise knowledge of material parameters is more and more important for improving crystal growth processes. Two important parameters are the contact (wetting) angle and the surface tension, determining meniscus shapes and surface-tension driven flows in a variety of methods (Czochralski, EFG, floating-zone, detached Bridgman growth). The sessile drop technique allows the measurement of both parameters simultaneously and has been used to measure the contact angles and the surface tension of Ge(1-x)Si(x) (0 less than or equal to x less than or equal to 1.3) alloys on various substrate materials. Fused quartz, Sapphire, glassy carbon, graphite, SiC, carbon-based aerogel, pyrolytic boron nitride (pBN), AIN, Si3N4, and polycrystalline CVD diamond were used as substrate materials. In addition, the effect of different cleaning procedures and surface treatments on the wetting behavior were investigated. Measurements were performed both under dynamic vacuum and gas atmospheres (argon or forming gas), with temperatures up to 1100 C. In some experiments, the sample was processed for longer times, up to a week, to investigate any changes of the contact angle and/or surface tension due to slow reactions with the substrate. For pure Ge, stable contact angles were found for carbon-based substrates and for pBN, for Ge(1-x)Si(x) only for pBN. The highest wetting angles were found for pBN substrates with angles around 170deg. For the surface tension of Ge, the most reliable values resulted in gamma(T) = (591- 0.077 (T-T(sub m)) 10(exp -3)N/m. The temperature dependence of the surface tension showed similar values for Ge(1-x)Si(x), around -0.08 x 10(exp -3)N/m K, and a compositional dependence of 2.2 x 10(exp -3)N/m at%Si.

Measurable characteristics of lysozyme crystal growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2005-01-01

The behavior of protein crystal growth is estimated from measurements performed at both the microscopic and molecular levels. In the absence of solutal flow, it was determined that a model that balances the macromolecular flux toward the crystal surface with the flux of the crystal surface well characterizes crystal growth observed using microscopic methods. Namely, it was determined that the model provides accurate estimates for the crystal-growth velocities upon evaluation of crystal-growth measurements obtained in time. Growth velocities thus determined as a function of solution supersaturation were further interpreted using established deterministic models. From analyses of crystal-growth velocities, it was found that the mode of crystal growth varies with respect to increasing solution supersaturation, possibly owing to kinetic roughening. To verify further the hypothesis of kinetic roughening, crystal growth at the molecular level was examined using atomic force microscopy (AFM). From the AFM measurements, it was found that the magnitude of surface-height fluctuations, h(x), increases with increasing solution supersaturation. In contrast, the estimated characteristic length, xi, decreases rapidly upon increasing solution supersaturation. It was conjectured that the magnitude of both h(x) and xi could possibly determine the mode of crystal growth. Although the data precede any exact theory, the non-critical divergence of h(x) and xi with respect to increasing solution supersaturation was nevertheless preliminarily established. Moreover, approximate models to account for behavior of both h(x) and xi are also presented.

Crystal Growth Rate Dispersion: A Predictor of Crystal Quality in Microgravity?

NASA Technical Reports Server (NTRS)

Kephart, Richard D.; Judge, Russell A.; Snell, Edward H.; vanderWoerd, Mark J.

2003-01-01

In theory macromolecular crystals grow through a process involving at least two transport phenomena of solute to the crystal surface: diffusion and convection. In absence of standard gravitational forces, the ratio of these two phenomena can change and explain why crystal growth in microgravity is different from that on Earth. Experimental evidence clearly shows, however, that crystal growth of various systems is not equally sensitive to reduction in gravitational forces, leading to quality improvement in microgravity for some crystals but not for others. We hypothesize that the differences in final crystal quality are related to crystal growth rate dispersion. If growth rate dispersion exists on Earth, decreases in microgravity, and coincides with crystal quality improvements then this dispersion is a predictor for crystal quality improvement. In order to test this hypothesis, we will measure growth rate dispersion both in microgravity and on Earth and will correlate the data with previously established data on crystal quality differences for the two environments. We present here the first crystal growth rate measurement data for three proteins (lysozyme, xylose isomerase and human recombinant insulin), collected on Earth, using hardware identical to the hardware to be used in microgravity and show how these data correlate with crystal quality improvements established in microgravity.

On geological interpretations of crystal size distributions: Constant vs. proportionate growth

USGS Publications Warehouse

Eberl, D.D.; Kile, D.E.; Drits, V.A.

2002-01-01

Geological interpretations of crystal size distributions (CSDs) depend on understanding the crystal growth laws that generated the distributions. Most descriptions of crystal growth, including a population-balance modeling equation that is widely used in petrology, assume that crystal growth rates at any particular time are identical for all crystals, and, therefore, independent of crystal size. This type of growth under constant conditions can be modeled by adding a constant length to the diameter of each crystal for each time step. This growth equation is unlikely to be correct for most mineral systems because it neither generates nor maintains the shapes of lognormal CSDs, which are among the most common types of CSDs observed in rocks. In an alternative approach, size-dependent (proportionate) growth is modeled approximately by multiplying the size of each crystal by a factor, an operation that maintains CSD shape and variance, and which is in accord with calcite growth experiments. The latter growth law can be obtained during supply controlled growth using a modified version of the Law of Proportionate Effect (LPE), an equation that simulates the reaction path followed by a CSD shape as mean size increases.

Connection between the growth rate distribution and the size dependent crystal growth

NASA Astrophysics Data System (ADS)

Mitrović, M. M.; Žekić, A. A.; IIić, Z. Z.

2002-07-01

The results of investigations of the connection between the growth rate dispersions and the size dependent crystal growth of potassium dihydrogen phosphate (KDP), Rochelle salt (RS) and sodium chlorate (SC) are presented. A possible way out of the existing confusion in the size dependent crystal growth investigations is suggested. It is shown that the size independent growth exists if the crystals belonging to one growth rate distribution maximum are considered separately. The investigations suggest possible reason for the observed distribution maxima widths, and the high data scattering on the growth rate versus the crystal size dependence.

Effect of Low-Concentration Polymers on Crystal Growth in Molecular Glasses: A Controlling Role for Polymer Segmental Mobility Relative to Host Dynamics.

PubMed

Huang, Chengbin; Powell, C Travis; Sun, Ye; Cai, Ting; Yu, Lian

2017-03-02

Low-concentration polymers can strongly influence crystal growth in small-molecule glasses, a phenomenon important for improving physical stability against crystallization. We measured the velocity of crystal growth in two molecular glasses, nifedipine (NIF) and o-terphenyl (OTP), each doped with four or five different polymers. For each polymer, the concentration was fixed at 1 wt % and a wide range of molecular weights was tested. We find that a polymer additive can strongly alter the rate of crystal growth, from a 10-fold reduction to a 10-fold increase. For a given polymer, increasing molecular weight slows down crystal growth and the effect saturates around DP = 100, where DP is the degree of polymerization. For all the systems studied, the polymer effect on crystal growth rate forms a master curve in the variable (T g,polymer - T g,host )/T cryst , where T g is the glass transition temperature and T cryst is the crystallization temperature. These results support the view that a polymer's effect on crystal growth is controlled by its segmental mobility relative to the host-molecule dynamics. In the proposed model, crystal growth rejects impurities and creates local polymer-rich regions, which must be traversed by host molecules to sustain crystal growth at rates determined by polymer segmental mobility. Our results do not support the view that host-polymer hydrogen bonding plays a controlling role in crystal growth inhibition.

Peculiar Features of Microstructure Formation and Microhardness Variations During Torsional Straining of Tantalum Specimens in Bridgman Anvils

NASA Astrophysics Data System (ADS)

Ditenberg, I. A.; Tymentsev, A. N.; Korznikov, A. V.

2015-04-01

Using the method of transmission electron microscopy, peculiar features of evolution of microstructure and variations in microhardness of Та are investigated under torsional loading in the Bridgman anvil as a function of plastic deformation at room temperature. A quantitative examination of grain and defect's structure of the material under study and the values of local internal stresses is performed in different loading stages. The mechanisms of formation of submicrocrystalline and nanostructured states are analyzed and so is the microstructure variation as a function of the defect-structure characteristics, strain level, and spacing from the axis of torsion.

Protein crystal growth in low gravity

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.

1990-01-01

The effect of low gravity on the growth of protein crystals and those parameters which will affect growth and crystal quality was studied. The proper design of the flight hardware and experimental protocols are highly dependent on understanding the factors which influence the nucleation and growth of crystals of biological macromolecules. Thus, those factors are investigated and the body of knowledge which has been built up for small molecule crystallization. These data also provide a basis of comparison for the results obtained from low-g experiments. The flows around growing crystals are detailed. The preliminary study of the growth of isocitrate lyase, the crystal morphologies found and the preliminary x ray results are discussed. The design of two apparatus for protein crystal growth by temperature control are presented along with preliminary results.

The study of single crystals for space processing and the effect of zero gravity

NASA Technical Reports Server (NTRS)

Lal, R. B.

1975-01-01

A study was undertaken to analyze different growth techniques affected by a space environment. Literature on crystal growth from melt, vapor phase and float zone was reviewed and the physical phenomena important for crystal growth in zero-gravity environment was analyzed. Recommendations for potential areas of crystal growth feasible for space missions are presented and a bibliography of articles in the area of crystal growth in general is listed.

Face-selective crystal growth behavior of L-aspartic acid in the presence of L-asparagine

NASA Astrophysics Data System (ADS)

Sato, Hiroyasu; Doki, Norihito; Yoshida, Saki; Yokota, Masaaki; Shimizu, Kenji

2016-02-01

The kinetic mechanism of L-asparagine (L-Asn) action on L-aspartic acid (L-Asp) crystal growth, namely the face-selective effect of L-Asn on the L-Asp crystal growth rate in each direction, was examined. In the a-axis direction, the effect of L-Asn on the L-Asp crystal growth rate was small. Enhancement and inhibition of L-Asp crystal growth, and interestingly the dissolution of the L-Asp crystal face, were observed in the b-axis direction, depending on the amount of L-Asn added. In the c-axis direction, the L-Asp crystal growth rate decreased with the increase in the amount of L-Asn added, and the experimental results were well fitted with a Langmuir adsorption isotherm. The study showed that there were crystal growth conditions where enhancement and inhibition, as well as inhibition and dissolution, coexisted in the presence of an additive with a structure similar to the growing crystal.

Delta L: An Apparatus for Measuring Macromolecular Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

In order to determine how macromolecule crystal quality improvement in microgravity is related to crystal growth characteristics, is was necessary to develop new hardware that could measure the crystal growth rates of a population of crystals growing under the same solution conditions. As crystal growth rate is defined as the change or delta in a defined dimension or length (L) of a crystal over time, the hardware was named Delta L. Delta L consists of fluids, optics, and data acquisition, sub-assemblies. Temperature control is provided for the crystal growth chamber. Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS). Delta L prototype hardware has been assembled. This paper will describe an overview of the design of Delta L and present preliminary crystal growth rate data.

Potential productivity benefits of float-zone versus Czochralski crystal growth

NASA Technical Reports Server (NTRS)

Abe, T.

1985-01-01

Efficient mass production of single-crystal silicon is necessary for the efficient silicon solar arrays needed in the coming decade. However, it is anticipated that there will be difficulty growing such volumes of crystals using conventional Czochralski (Cz) methods. While the productivity of single crystals might increase with a crystal diameter increase, there are two obstacles to the mass production of large diameter Czochralski crystals, the long production cycle due to slow growth rate and the high heat requirements of the furnaces. Also counterproductive would be the large resistivity gradient along the growth direction of the crystals due to impurity concentration. Comparison between Float zone (FZ) and Cz crystal growth on the basis of a crystal 150 mm in diameter is on an order of two to four times in favor of the FZ method. This advantage results from high growth rates and steady-state growth while maintaining a dislocation-free condition and impurity segregation.

Optical Diagnostics of Solution Crystal Growth

NASA Technical Reports Server (NTRS)

Kim, Yongkee; Reddy, B. R.; George, T. G.; Lal, R. B.

1996-01-01

Non-contact optical techniques such as, optical heterodyne, ellipsometry and interferometry, for real time in-situ monitoring of solution crystal growth are demonstrated. Optical heterodyne technique has the capability of measuring the growth rate as small as 1A/sec. In a typical Michelson interferometer set up, the crystal is illuminated by a Zeeman laser with frequency omega(sub 1) and the reference beam with frequency omega(sub 2). As the crystal grows, the phase of the rf signal changes with respect to the reference beam and this phase change is related to the crystal growth rate. This technique is demonstrated with two examples: (1) by measuring the copper tip expansion/shrinkage rate and (2) by measuring the crystal growth rate of L-Arginine Phosphate (LAP). The first test shows that the expansion/shrinkage rate of copper tip was fast in the beginning, and gets slower as the expansion begins to stabilize with time. In crystal growth, the phase change due the crystal growth is measured using a phase meter and a strip chart recorder. Our experimental results indicate a varied growth rate from 69.4 to 92.6A per sec. The ellipsometer is used to study the crystal growth interface. From these measurements and a theoretical modeling of the interface, the various optical parameters can be deduced. Interferometry can also be used to measure the growth rate and concentration gradient in the vicinity of the crystal.

Hopper Growth of Salt Crystals.

PubMed

Desarnaud, Julie; Derluyn, Hannelore; Carmeliet, Jan; Bonn, Daniel; Shahidzadeh, Noushine

2018-06-07

The growth of hopper crystals is observed for many substances, but the mechanism of their formation remains ill understood. Here we investigate their growth by performing evaporation experiments on small volumes of salt solutions. We show that sodium chloride crystals that grow very fast from a highly supersaturated solution form a peculiar form of hopper crystal consisting of a series of connected miniature versions of the original cubic crystal. The transition between cubic and such hopper growth happens at a well-defined supersaturation where the growth rate of the cubic crystal reaches a maximum (∼6.5 ± 1.8 μm/s). Above this threshold, the growth rate varies as the third power of supersaturation, showing that a new mechanism, controlled by the maximum speed of surface integration of new molecules, induces the hopper growth of cubic crystals in cascade.

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.

Effect of precipitation inhibitors on indomethacin supersaturation maintenance: mechanisms and modeling.

PubMed

Patel, Dhaval D; Anderson, Bradley D

2014-05-05

This study quantitatively explores the mechanisms underpinning the effects of model pharmaceutical polymeric precipitation inhibitors (PPIs) on the crystal growth and, in turn, maintenance of supersaturation of indomethacin, a model poorly water-soluble drug. A recently developed second-derivative UV spectroscopy method and a first-order empirical crystal growth model were used to determine indomethacin crystal growth rates in the presence of model PPIs. All three model PPIs including HP-β-CD, PVP, and HPMC inhibited indomethacin crystal growth at both high and low degrees of supersaturation (S). The bulk viscosity changes in the presence of model PPIs could not explain their crystal growth inhibitory effects. At 0.05% w/w, PVP (133-fold) and HPMC (28-fold) were better crystal growth inhibitors than HP-β-CD at high S. The inhibitory effect of HP-β-CD on the bulk diffusion-controlled indomethacin crystal growth at high S was successfully modeled using reactive diffusion layer theory, which assumes reversible complexation in the diffusion layer. Although HP-β-CD only modestly inhibited indomethacin crystal growth at either high S (∼15%) or low S (∼2-fold), the crystal growth inhibitory effects of PVP and HPMC were more dramatic, particularly at high S (0.05% w/w). The superior crystal growth inhibitory effects of PVP and HPMC as compared with HP-β-CD at high S were attributed to a change in the indomethacin crystal growth rate-limiting step from bulk diffusion to surface integration. Indomethacin crystal growth inhibitory effects of all three model PPIs at low S were attributed to retardation of the rate of surface integration of indomethacin, a phenomenon that may reflect the adsorption of PPIs onto the growing crystal surface. The quantitative approaches outlined in this study should be useful in future studies to develop tools to predict supersaturation maintenance effects of PPIs.

Control of heat transfer in continuous-feeding Czochralski-silicon crystal growth with a water-cooled jacket

NASA Astrophysics Data System (ADS)

Zhao, Wenhan; Liu, Lijun

2017-01-01

The continuous-feeding Czochralski method is an effective method to reduce the cost of single crystal silicon. By promoting the crystal growth rate, the cost can be reduced further. However, more latent heat will be released at the melt-crystal interface under a high crystal growth rate. In this study, a water-cooled jacket was applied to enhance the heat transfer at the melt-crystal interface. Quasi-steady-state numerical calculation was employed to investigate the impact of the water-cooled jacket on the heat transfer at the melt-crystal interface. Latent heat released during the crystal growth process at the melt-crystal interface and absorbed during feedstock melting at the feeding zone was modeled in the simulations. The results show that, by using the water-cooled jacket, heat transfer in the growing crystal is enhanced significantly. Melt-crystal interface deflection and thermal stress increase simultaneously due to the increase of radial temperature at the melt-crystal interface. With a modified heat shield design, heat transfer at the melt-crystal interface is well controlled. The crystal growth rate can be increased by 20%.

Crystal growth and annealing for minimized residual stress

DOEpatents

Gianoulakis, Steven E.

2002-01-01

A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF.sub.2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing.

An assessment of calcite crystal growth mechanisms based on crystal size distributions

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.; Hoch, A.R.; Reddy, M.M.

2000-01-01

Calcite crystal growth experiments were undertaken to test a recently proposed model that relates crystal growth mechanisms to the shapes of crystal size distributions (CSDs). According to this approach, CSDs for minerals have three basic shapes: (1) asymptotic, which is related to a crystal growth mechanism having constant-rate nucleation accompanied by surface-controlled growth; (2) lognormal, which results from decaying-rate nucleation accompanied by surface-controlled growth; and (3) a theoretical, universal, steady-state curve attributed to Ostwald ripening. In addition, there is a fourth crystal growth mechanism that does not have a specific CSD shape, but which preserves the relative shapes of previously formed CSDs. This mechanism is attributed to supply-controlled growth. All three shapes were produced experimentally in the calcite growth experiments by modifying nucleation conditions and solution concentrations. The asymptotic CSD formed when additional reactants were added stepwise to the surface of solutions that were supersaturated with respect to calcite (initial Ω = 20, where Ω = 1 represents saturation), thereby leading to the continuous nucleation and growth of calcite crystals. Lognormal CSDs resulted when reactants were added continuously below the solution surface, via a submerged tube, to similarly supersaturated solutions (initial Ω = 22 to 41), thereby leading to a single nucleation event followed by surface-controlled growth. The Ostwald CSD resulted when concentrated reactants were rapidly mixed, leading initially to high levels of supersaturation (Ω >100), and to the formation and subsequent dissolution of very small nuclei, thereby yielding CSDs having small crystal size variances. The three CSD shapes likely were produced early in the crystallization process, in the nanometer crystal size range, and preserved during subsequent growth. Preservation of the relative shapes of the CSDs indicates that a supply-controlled growth mechanism was established and maintained during the constant-composition experiments. CSDs having shapes intermediate between lognormal and Ostwald also were generated by varying the initial levels of supersaturation (initial Ω = 28.2 to 69.2) in rapidly mixed solutions. Lognormal CSDs were observed for natural calcite crystals that are found in septarian concretions occurring in southeastern Colorado. Based on the model described above, these CSDs indicate initial growth by surface control, followed by supply-controlled growth. Thus, CSDs may be used to deduce crystal growth mechanisms from which geologic conditions early in the growth history of a mineral can be inferred. Conversely, CSD shape can be predicted during industrial crystallization by applying the appropriate conditions for a particular growth mechanism.

In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

NASA Astrophysics Data System (ADS)

Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

2014-09-01

The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

The control of ice crystal growth and effect on porous structure of konjac glucomannan-based aerogels.

PubMed

Ni, Xuewen; Ke, Fan; Xiao, Man; Wu, Kao; Kuang, Ying; Corke, Harold; Jiang, Fatang

2016-11-01

Konjac glucomannan (KGM)-based aerogels were prepared using a combination of sol-gel and freeze-drying methods. Preparation conditions were chosen to control ice crystal growth and aerogel structure formation. The ice crystals formed during pre-freezing were observed by low temperature polarizing microscopy, and images of aerogel pores were obtained by scanning electron microscopy. The size of ice crystals were calculated and size distribution maps were drawn, and similarly for aerogel pores. Results showed that ice crystal growth and aerogel pore sizes may be controlled by varying pre-freezing temperatures, KGM concentration and glyceryl monostearate concentration. The impact of pre-freezing temperatures on ice crystal growth was explained as combining ice crystal growth rate with nucleation rate, while the impacts of KGM and glyceryl monostearate concentration on ice crystal growth were interpreted based on their influences on sol network structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Growth of benzil crystals by vertical dynamic gradient freeze technique in a transparent furnace

NASA Astrophysics Data System (ADS)

Lan, C. W.; Song, C. R.

1997-09-01

The vertical dynamic gradient freeze technique using a transparent furnace was applied to the growth of benzil single crystals. A flat-bottom ampoule with a <0001> seed was used for growth. During crystal growth, dynamic heating profiles were controlled through a computer, and the growth interface was recorded by a CCD camera. Computer simulation was also conducted, and the calculated convex interface and dynamic growth rate were consistent with the observed ones for various growth conditions. Conditions for growing single crystals were also determined, and they were mainly limited by constitutional supercooling. As the grown crystals were clear in appearance, their optical absorption spectra were insensitive to growth conditions and post-annealing.

Protein crystal growth tray assembly

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor); Miller, Teresa Y. (Inventor)

1992-01-01

A protein crystal growth tray assembly includes a tray that has a plurality of individual crystal growth chambers. Each chamber has a movable pedestal which carries a protein crystal growth compartment at an upper end. The several pedestals for each tray assembly are ganged together for concurrent movement so that the solutions in the various pedestal growth compartments can be separated from the solutions in the tray's growth chambers until the experiment is to be activated.

Rate limits in silicon sheet growth - The connections between vertical and horizontal methods

NASA Technical Reports Server (NTRS)

Thomas, Paul D.; Brown, Robert A.

1987-01-01

Meniscus-defined techniques for the growth of thin silicon sheets fall into two categories: vertical and horizontal growth. The interactions of the temperature field and the crystal shape are analyzed for both methods using two-dimensional finite-element models which include heat transfer and capillarity. Heat transfer in vertical growth systems is dominated by conduction in the melt and the crystal, with almost flat melt/crystal interfaces that are perpendicular to the direction of growth. The high axial temperature gradients characteristic of vertical growth lead to high thermal stresses. The maximum growth rate is also limited by capillarity which can restrict the conduction of heat from the melt into the crystal. In horizontal growth the melt/crystal interface stretches across the surface of the melt pool many times the crystal thickness, and low growth rates are achievable with careful temperature control. With a moderate axial temperature gradient in the sheet a substantial portion of the latent heat conducts along the sheet and the surface of the melt pool becomes supercooled, leading to dendritic growth. The thermal supercooling is surpressed by lowering the axial gradient in the crystal; this configuration is the most desirable for the growth of high quality crystals. An expression derived from scaling analysis relating the growth rate and the crucible temperature is shown to be reliable for horizontal growth.

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

DOE PAGES

Godinho, Jose R. A.; Stack, Andrew G.

2015-03-30

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

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

Godinho, Jose R. A.; Stack, Andrew G.

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

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

NASA Astrophysics Data System (ADS)

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

2012-02-01

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

CePd2Ga3 and CePd2Zn3 - Kondo lattices and magnetic behaviour

NASA Astrophysics Data System (ADS)

Bartha, A.; Vališka, M.; Míšek, M.; Proschek, P.; Kaštil, J.; Dušek, M.; Sechovský, V.; Prokleška, J.

2018-05-01

We report the single crystal properties of CePd2Zn3 and CePd2Ga3 compounds. The compounds were prepared by Bridgman method in high-frequency induction furnace. Both compounds adopt the hexagonal PrNi2Al3-type structure with a = 5.3914(2) Å, c = 4.3012(2) Å for CePd2Zn3 and a = 5.4106(8) Å, c = 4.2671(8) Å for CePd2Ga3, respectively. CePd2Zn3 orders antiferromagnetically below TN = 1.9 K. Magnetoresistance measurements revealed a crossover at Bc = 0.95 T. CePd2Ga3 orders ferromagnetically at TC = 6.7 K. Applied hydrostatic pressure reduces the value of the Curie-temperature (rate ∂TC / ∂ p = 0.9 K GPa -1) down to 3.9 K at 3.2 GPa. Both compounds display a strong magnetocrystalline anisotropy with easy axis of magnetization perpendicular to the c-axis in the hexagonal lattice.

Thallous chalcogenide (Tl 6I 4Se) for radiation detection at X-ray and γ-ray energies

NASA Astrophysics Data System (ADS)

Liu, Zhifu; Peters, John A.; Wessels, Bruce W.; Johnsen, Simon; Kanatzidis, Mercouri G.

2011-12-01

The optical and charge transport properties of the thallous chalcogenide compound Tl6I4Se were characterized. The semiconductor crystals are grown by the modified Bridgman method. We have measured the refractive index, and absorption coefficient of the compound ranging from 300 to 1500 nm by analysis of the UV-vis-near IR transmission and reflection spectra. The band gap is 1.8 eV. For the evaluation of detector performance, the mobility-lifetime products for both the electron and hole carriers were measured. Tl6I4Se has mobility-lifetime products of 7.1×10-3 and 5.9×10-4 cm2/V for electron and hole carriers, respectively, which are comparable to those of Cd0.9Zn0.1Te. The γ-ray spectrum for a Tl6I4Se detector was measured. Its response to the 122 keV of 57Co source is comparable to that of Cd0.9Zn0.1Te.

Fast growth of n-type 4H-SiC bulk crystal by gas-source method

NASA Astrophysics Data System (ADS)

Hoshino, Norihiro; Kamata, Isaho; Tokuda, Yuichiro; Makino, Emi; Kanda, Takahiro; Sugiyama, Naohiro; Kuno, Hironari; Kojima, Jun; Tsuchida, Hidekazu

2017-11-01

Fast growth of n-type 4H-SiC crystals was attempted using a high-temperature gas-source method. High growth rates exceeding 9 mm/h were archived at a seed temperature of 2550 °C, although the formation of macro-step bunching caused doping fluctuation and voids in the grown crystal. We investigated a trade-off between growth-rate enhancement and macro-step formation and how to improve the trade-off. By controlling the growth conditions, the growth of highly nitrogen-doped 4H-SiC crystals without the doping fluctuation and void formation were accomplished under a high growth rate exceeding 3 mm/h, maintaining the density of threading screw dislocations in the same level with the seed crystal. The influence of growth parameters on nitrogen incorporations into grown crystals was also surveyed.

Maintenance of supersaturation I: indomethacin crystal growth kinetic modeling using an online second-derivative ultraviolet spectroscopic method.

PubMed

Patel, Dhaval D; Joguparthi, Vijay; Wang, Zeren; Anderson, Bradley D

2011-07-01

Formulations that produce supersaturated solutions after their oral administration have received increased attention as a means to improve bioavailability of poorly water-soluble drugs. Although it is widely recognized that excipients can prolong supersaturation, the mechanisms by which these beneficial effects are realized are generally unknown. Difficulties in separately measuring the kinetics of nucleation and crystal growth have limited progress in understanding the mechanisms by which excipients contribute to the supersaturation maintenance. This paper describes the crystal growth kinetic modeling of indomethacin, a poorly water-soluble drug, from supersaturated aqueous suspensions using a newly developed, online second-derivative ultraviolet spectroscopic method. The apparent indomethacin equilibrium solubility after crystal growth at a high degree of supersaturation (S=6) was approximately 55% higher than the indomethacin equilibrium solubility determined prior to growth, which was attributed to the deposition of a higher energy indomethacin form on the seed crystals. The indomethacin crystal growth kinetics (S=6) was of first order. By comparing the mass transfer coefficients from indomethacin dissolution and crystal growth, it was shown that the indomethacin crystal growth kinetics at S=6 was bulk diffusion controlled. The change in indomethacin seed crystal size distribution before and after crystal growth was determined and modeled using a mass-balance relationship. Copyright © 2011 Wiley-Liss, Inc. and the American Pharmacists Association

Crystal growth mechanisms in miarolitic cavities in the Lake George ring complex and vicinity, Colorado

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

1999-01-01

The Crystal Peak area of the Pikes Peak batholith, near Lake George in central Colorado, is world-renowned for its crystals of amazonite (the blue-green variety of microcline) and smoky quartz. Such crystals, collected from individual miarolitic pegmatites, have a remakably small variation in crystal size within each pegmatite, and the shapes of plots of their crystal size distributions (CSDs) are invariably lognormal or close to lognormal in all cases. These observations are explained by a crystal growth mechanism that was governed initially by surface-controlled kinetics, during which crystals tended to grow larger in proportion to their size, thereby establishing lognormal CSDs. Surface-controlled growth was followed by longer periods of supply controlled growth, during which growth rate was predominantly size-independent, consequently preserving the lognormal shapes of the CSDs and the small size variation. The change from surface- to supply controlled growth kinetics may have resulted from an increasing demand for nutrients that exceeded diffusion limitations of the system. The proposed model for crystal growth in this locality appears to be common in the geologic record, and can be used with other information, such as isotopic data, to deduce physico-chemical conditions during crystal formation.