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At least 253 records · Page 14

Characterization of Surface Features in Detached Grown GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. It is commonly understood that the main factors that promote the occurrence of detached growth include: high contact angle between the melt and the crucible material, high growth angle, and a pressure difference between the annular gap around the solid below the melt and the volume above the melt along the meniscus. These parameters were varied in Bridgman growth experiments to determine the conditions required to achieve detached growth terrestrially in Ge and GeSi alloys. These experiments are in preparation for experiments on the International Space Station (ISS). The detailed objectives of the flight experiments and a description of the growth methods employed are the subject of another presentation at this Conference. Detached crystals were achieved repeatedly in pyrolytic boron nitride ampoules when a pressure difference was employed. All crystals, except for those grown in fused silica ampoules, were easily removed from their containers, however, this fact alone is not sufficient to infer detached growth. Detachment was verified by comparing profilometer measurements of the radius of the samples with observations of the sample surfaces using optical and electron microscopy. The surfaces of the attached areas of the crystals had the same shape and surface texture as the interior crucible wall. Regions of detached growth contained many unique features and crystal facets could usually be observed. Several of these surface features have been correlated with mechanisms of detachment or free-surface growth and others to processing events or conditions.

Cobb, S. D.↗

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

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.

Huang, YU↗

Dopant segregation in YAG single crystal fibers grown by the laser heated pedestal growth technique

In this work, we report self-segregation of dopants in a crystal matrix within a single crystal (SC) fiber. Neodymium and holmium-doped yttrium aluminum garnet (YAG) fibers were grown using the Laser Heated Pedestal Growth (LHPG) technique and cross-sectional dopant concentration was measured using electron-probe micro-analysis. It was observed that the degree of auto-segregation of the rare-earth dopant depended on the difference in ionic size of the dopant ion and the Y 3+ ion in the YAG matrix. While holmium showed little tendency to self-segregate, the concentration of neodymium ions varied as much as 25% across the cross-section of the fiber. Strong correlation between the dopant concentration profile and fiber draw speed was also demonstrated. Since the local refractive index depends on the concentration of dopants, a refractive index profile can be achieved by a dopant profile across the fiber cross-section. Engineered index profiles can be realized by varying growth conditions, dopants, crystal matrix, etc. Such an approach is promising in applications such as the development of monolithic SC fibers with graded-index profiles.

36 MATERIALS SCIENCE↗

Study of LPE methods for growth of InGaAsP/InP CW lasers

Two methods for liquid phase growth of InGaAsP/InP lasers were studied. Single phase growth, based on saturated melts and 5 C supercooling, was compared to two phase growth excess InP and 20 C nominal supercooling. Substrates cut on the (100) plane were used, and morphology in both cases was excellent and comparable to that obtainable in AlGaAs materials. A high degree of reproducibility was obtained in the materials grown by the two phased method, which is therefore presently preferred for the preparation of laser material. A refractive index step of 0.28 and an index n = 3.46 were obtained for In.81Ga.19As,5P5 lasing at 1.3 microns. Oxide-stripe lasers with typical room temperature cw threshold currents of 180 mA were obtained and some of them showed single mode behavior without lateral cavity modifications. COntinuous operation of 800 h at room temperature was obtained without noticeable degradation.

Ladany, I.↗

Shuttle Mission STS-50: Orbital Processing of High-Quality CdTe Compound Semiconductors Experiment: Final Flight Sample Characterization Report

The Orbital Processing of High-Quality Doped and Alloyed CdTe Compound Semiconductors program was initiated to investigate, quantitatively, the influences of gravitationally dependent phenomena on the growth and quality of bulk compound semiconductors. The objective was to improve crystal quality (both structural and compositional) and to better understand and control the variables within the crystal growth production process. The empirical effort entailed the development of a terrestrial (one-g) experiment baseline for quantitative comparison with microgravity (mu-g) results. This effort was supported by the development of high-fidelity process models of heat transfer, fluid flow and solute redistribution, and thermo-mechanical stress occurring in the furnace, safety cartridge, ampoule, and crystal throughout the melting, seeding, crystal growth, and post-solidification processing. In addition, the sensitivity of the orbital experiments was analyzed with respect to the residual microgravity (mu-g) environment, both steady state and g-jitter. CdZnTe crystals were grown in one-g and in mu-g. Crystals processed terrestrially were grown at the NASA Ground Control Experiments Laboratory (GCEL) and at Grumman Aerospace Corporation (now Northrop Grumman Corporation). Two mu-g crystals were grown in the Crystal Growth Furnace (CGF) during the First United States Microgravity Laboratory Mission (USML-1), STS-50, June 24 - July 9, 1992.

Larson, David J.↗

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

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.

Ma, Nancy↗

Silicon web process development

Silicon dendritic web, a single crystal ribbon shaped during growth by crystallographic forces and surface tension (rather than dies), is a highly promising base material for efficient low cost solar cells. The form of the product smooth, flexible strips 100 to 200 microns thick, conserves expensive silicon and facilitates automation of crystal growth and the subsequent manufacturing of solar cells. These characteristics, coupled with the highest demonstrated ribbon solar cell efficiency-15.5%-make silicon web a leading candidate to achieve, or better, the 1986 Low Cost Solar Array (LSA) Project cost objective of 50 cents per peak watt of photovoltaic output power. The main objective of the Web Program, technology development to significantly increase web output rate, and to show the feasibility for simultaneous melt replenishment and growth, have largely been accomplished. Recently, web output rates of 23.6 sq cm/min, nearly three times the 8 sq cm/min maximum rate of a year ago, were achieved. Webs 4 cm wide or greater were grown on a number of occassions.

Duncan, C. S.↗

New outlook on control of crystalline and chemical perfection during growth of silicon

Significant progress has been made in our understanding of the Czochralski crystal growth process with the realization that the incorporation of oxygen into silicon is directly related to the internal gettering capability of wafers during device fabrication. It was also recognized that the electronic properties exhibited by silicon during various stages of device fabrication were significantly affected by the thermal history of the silicon during the post-growth cool-down period. Turbulent melt convection, induced by unavoidable destabilizing thermal gradients, was found to interfere with homogeneous dopant (and oxygen) incorporation and to influence markedly the dynamics of nonequilibrium point defects in the solidified silicon matrix during the cool-down period. In view of the unavoidability of destabilizing thermal gradients in conventional crystal growth configurations, melt stabilization through the application of magnetic fields is generally considered a viable approach. Control of heat input to the melt through heat pipe systems, as used during growth of germanium, cannot be applied to industrial growth of silicon. Recent studies have shown that heat exchange systems located coaxially about a growing crystal can be used to stabilize and control not only heat transfer in the grown crystal, but also in the melt adjacent to the solidification interface.

Witt, A. F.↗

Dendritic Alloy Solidification Experiment (DASE)

A space experiment, and supporting ground-based research, is proposed to study the microstructural evolution in free dendritic growth from a supercooled melt of the transparent model alloy succinonitrile-acetone (SCN-ACE). The research is relevant to equiaxed solidification of metal alloy castings. The microgravity experiment will establish a benchmark for testing of equiaxed dendritic growth theories, scaling laws, and models in the presence of purely diffusive, coupled heat and solute transport, without the complicating influences of melt convection. The specific objectives are to: determine the selection of the dendrite tip operating state, i.e. the growth velocity and tip radius, for free dendritic growth of succinonitrile-acetone alloys; determine the growth morphology and sidebranching behavior for freely grown alloy dendrites; determine the effects of the thermal/solutal interactions in the growth of an assemblage of equiaxed alloy crystals; determine the effects of melt convection on the free growth of alloy dendrites; measure the surface tension anisotropy strength of succinon itrile -acetone alloys establish a theoretical and modeling framework for the experiments. Microgravity experiments on equiaxed dendritic growth of alloy dendrites have not been performed in the past. The proposed experiment builds on the Isothermal Dendritic Growth Experiment (IDGE) of Glicksman and coworkers, which focused on the steady growth of a single crystal from pure supercooled melts (succinonitrile and pivalic acid). It also extends the Equiaxed Dendritic Solidification Experiment (EDSE) of the present investigators, which is concerned with the interactions and transients arising in the growth of an assemblage of equiaxed crystals (succinonitrile). However, these experiments with pure substances are not able to address the issues related to coupled heat and solute transport in growth of alloy dendrites.

Beckermann, C.↗

Analysis of low gravity tolerance of model experiments for space station: Preliminary results for directional solidification

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.

Alexander, J. Iwan D.↗

Large area sheet task. Advanced dendritic web growth development

The development of a silicon dendritic web growth machine is discussed. Several refinements to the sensing and control equipment for melt replenishment during web growth are described and several areas for cost reduction in the components of the prototype automated web growth furnace are identified. A circuit designed to eliminate the sensitivity of the detector signal to the intensity of the reflected laser beam used to measure melt level is also described. A variable speed motor for the silicon feeder is discussed which allows pellet feeding to be accomplished at a rate programmed to match exactly the silicon removed by web growth.

Duncan, C. S.↗

Advanced Czochralski silicon growth technology for photovoltaic modules

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

Daud, T.↗

Analysis of Experimental Ice Accretion Data and Assessment of a Thermodynamic Model During Ice Crystal Icing

This paper evaluates a thermodynamic ice crystal icing model that has been previously presented to describe the possible mechanisms of icing within the core of a turbofan jet engine. The model functions between two distinct ice accretions based on a surface energy balance: freeze-dominated icing and melt-dominated icing. Freeze-dominated icing occurs when liquid water (from melted ice crystals) freezes and accretes on a surface along with the existing ice of the impinging water and ice mass. This freeze-dominated icing is characterized as having strong adhesion to the surface. The amount of ice accretion is partially dictated by a freeze fraction, which is the fraction of impinging liquid water that freezes. Melt-dominated icing occurs as unmelted ice on a surface accumulates. This melt-dominated icing is characterized by weakly bonded surface adhesion. The amount of ice accumulation is partially dictated by a melt fraction, which is the fraction of impinging ice crystals that melts. Experimentally observed ice growth rates suggest that only a small fraction of the impinging ice remains on the surface, implying a mass loss mechanism such as splash, runback, bounce, or erosion. The fraction of mass loss must be determined in conjunction with the fraction of freezing liquid water or fraction of melting ice on an icing surface for a given ice growth rate. This mass loss parameter, however, along with the freeze fraction and melt fraction, are the only experimental parameters that are currently not measured directly. Using icing growth rates from ice crystal icing experiments, a methodology that has been previously proposed is used to determine these unknown parameters. This work takes ice accretion data from tests conducted by the National Aeronautics and Space Administration (NASA) at the Glenn Research Center in 2018 that examined the fundamental physics of ice crystal icing. This paper continues evaluation of the thermodynamic model from a previous effort, with additions to the model that account for sub-freezing temperatures that have been observed at the leading edge of the airfoil during icing. The predicted temperatures were generally in good agreement with measured temperatures. Other key findings include the total wet-bulb temperature being a good first order indicator of whether icing is freeze-dominated (sub-freezing values) or melt-dominated (above freezing). Maximum sticking efficiency values, the fraction of impinging mass that adheres to a surface, was calculated to be about 0.2, and retained this maximum value for a range of melt ratios (0.3 to 0.65 and possibly higher), which is defined as the ratio of liquid water content to total water content. Higher air velocities reduced the maximum sticking efficiency and shifted the icing regime to higher melt ratio values. Finally, the leading edge ice accretion angle was found to be related to ice growth (lower growth rates for smaller angles) and melt ratio (smaller melt ratios resulted in smaller angles, likely due to erosion effects).

Ice-Crystal Icing↗

Effect of melt shearing on D -mannitol crystal twisting in the presence of small molecule and macromolecular additives

Here, many molecular crystals grow as twisted lamellae from the melt when the driving force is high, but the mechanisms governing the spontaneous formation of helicoidal crystallites are varied and those operative in particular cases are difficult to identify. Polyvinylpyrrolidone (PVP) induces the crystallization of D-mannitol as banded spherulites comprised of twisted fibrils emanating radially from spherulite nucleation centers. The molecular weight of the PVP phase affects the twisting pitch, P, (rotation of the crystallite by 180°), in D-mannitol thin films crystallized from the melt. At a relatively high crystallization temperature (T c =130°C), P was sensitive to the PVP molecular weight, ranging from 390±20 μm for D-mannitol films incorporating 15 wt% 10 kDa PVP to 20±3 μm for the same weight of 1300 kDa PVP. Magnitudes of complex viscosities, |η*|, of D-mannitol/PVP melts measured via small-amplitude oscillatory shearing were strongly dependent on the PVP molecular weight, but were not correlated to P(T). Instead, P was sensitive to the dynamic PVP chain conformation during D-mannitol crystallization. Under steady torsional shear, P decreased from~30 μm to~8μm with increasing shear rates from 0.01 to 100 s -1 for D-mannitol films crystallized at 130°C in the presence of 15 wt% 10 or 1300 kDa PVP. Shear forces decrease the entanglement density of polymer chains while orienting the chains along the stream lines of the viscometric flow, indicating that the conformations of macromolecular additives can affect the pitch of banded spherulites. By contrast, P in D-mannitol twisted by D-sorbitol was independent of shear rate.

36 MATERIALS SCIENCE↗

Dynamics of a Persistent Insulator-to-Metal Transition in Strained Manganite Films

Transition metal oxides possess complex free-energy surfaces with competing degrees of freedom. Photoexcitation allows shaping of such rich energy landscapes. In epitaxially strained La 0.67 Ca 0.33 MnO 3 , optical excitation with a sub-100-fs pulse above 2 mJ/cm 2 leads to a persistent metallic phase below 100 K. Here, using single-shot optical and terahertz spectroscopy, we show that this phase transition is a multistep process. We conclude that the phase transition is driven by partial charge-order melting, followed by growth of the persistent metallic phase on longer timescales. A time-dependent Ginzburg-Landau model can describe the fast dynamics of the reflectivity, followed by longer timescale in-growth of the metallic phase.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Silicon ribbon growth by a capillary action shaping technique

The crystal growth method described is a capillary action shaping technique. Meniscus shaping for the desired ribbon geometry occurs at the vertex of a wettable die. As ribbon growth depletes the melt meniscus, capillary action supplies replacement material. A capillary die is so designed that the bounding edges of the die top are not parallel or concentric with the growing ribbon. The new dies allow a higher melt meniscus with concomitant improvements in surface smoothness and freedom from SiC surface particles, which can degrade perfection.

Schwuttke, G. H.↗