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At least 19 records

Segregation Coefficients of Impurities in Selenium by Zone Refining

The purification of Se by zone refining process was studied. The impurity solute levels along the length of a zone-refined Se sample were measured by spark source mass spectrographic analysis. By comparing the experimental concentration levels with theoretical curves the segregation coefficient, defined as the ratio of equilibrium concentration of a given solute in the solid to that in the liquid, k = x(sub s)/x(sub l) for most of the impurities in Se are found to be close to unity, i.e., between 0.85 and 1.15, with the k value for Si, Zn, Fe, Na and Al greater than 1 and that for S, Cl, Ca, P, As, Mn and Cr less than 1. This implies that a large number of passes is needed for the successful implementation of zone refining in the purification of Se.

Su, Ching-Hua↗

Contactless heater floating zone refining and crystal growth

Floating zone refining or crystal growth is carried out by providing rapid relative rotation of a feed rod and finish rod while providing heat to the junction between the two rods so that significant forced convection occurs in the melt zone between the two rods. The forced convection distributes heat in the melt zone to allow the rods to be melted through with a much shorter melt zone length than possible utilizing conventional floating zone processes. One of the rods can be rotated with respect to the other, or both rods can be counter-rotated, with typical relative rotational speeds of the rods ranging from 200 revolutions per minute (RPM) to 400 RPM or greater. Zone refining or crystal growth is carried out by traversing the melt zone through the feed rod.

Kou, Sindo↗

Zone-refining encapsulated semiconductors

Reflector directs intense, sharply focused heat precisely where it is needed for zone-refining semiconductor materials. Reflector is especially suited for compound semiconductors which must be sealed inside capsule to prevent vaporizing during zone refining. Device is flattened toroid with elliptical-cross-section, much like horizontal partly-inflated inner tube.

Davidson, M. C.↗

Laser furnace and method for zone refining of semiconductor wafers

A method of zone refining a crystal wafer (116 FIG. 1) comprising the steps of focusing a laser beam to a small spot (120) of selectable size on the surface of the crystal wafer (116) to melt a spot on the crystal wafer, scanning the small laser beam spot back and forth across the surface of the crystal wafer (116) at a constant velocity, and moving the scanning laser beam across a predetermined zone of the surface of the crystal wafer (116) in a direction normal to the laser beam scanning direction and at a selectible velocity to melt and refine the entire crystal wafer (116).

Griner, Donald B.↗

Laser Vacuum Furnace for Zone Refining

Laser beam scanned to produce moving melt zone. Experimental laser vacuum furnace scans crystalline wafer with high-power CO2-laser beam to generate precise melt zone with precise control of temperature gradients around zone. Intended for zone refining of silicon or other semiconductors in low gravity, apparatus used in normal gravity.

Griner, D. B.↗

A graphical treatment of combined evaporation and segregation contributions to impurity profiles for zone-refining in vacuum

Impurity concentration profiles have been calculated for zone-refining when both segregation and evaporation of impurities are operative, assuming a uniform initial concentration. Graphic profiles are presented for selected values of effective segregation coefficient k, effective evaporation coefficient g, and number of zone passes n. Some examples of impurity profiles for float-zoned silicon are also presented.

Ciszek, T. F.↗

Traveling Molten Zone Refining Process Development for Innovative Fuel Cycle Solutions

This ARPA-E ONWARDS project successfully developed and demonstrated an innovative immiscibility zone refining process for separating actinides from active fission products in metallic nuclear fuel applications. The technology addresses a critical challenge in advanced nuclear fuel cycles by providing a high-throughput, low-waste alternative to conventional electrorefining.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Zone Refining by Laser

System developed for studying use of laser beam for zone-refining semiconductors and metals. Specimen scanned with focused CO2 laser beam in such way that thin zone of molten material moves along specimen sweeps impurities with it. Zone-melting system comprises microcomputer, laser, electromechanical and optical components for beam control, vacuum chamber that holds specimen, and sensor for determining specimen temperature.

Griner, D. B.↗

Solar energy concentrator system for crystal growth and zone refining in space

The technological feasibility of using solar concentrators for crystal growth and zone refining in space has been performed. Previous studies of space-deployed solar concentrators were reviewed for their applicability to materials processing and a new state-of-the-art concentrator-receiver radiation analysis was developed. The radiation analysis is in the form of a general purpose computer program. It was concluded from this effort that the technology for fabricating, orbiting and deploying large solar concentrators has been developed. It was also concluded that the technological feasibility of space processing materials in the focal region of a solar concentrator depends primarily on two factors: (1) the ability of a solar concentrator to provide sufficient thermal energy for the process and (2) the ability of a solar concentrator to provide a thermal environment that is conductive to the processes of interest. The analysis indicate that solar concentrators can satisfactorily provide both of these factors.

Mcdermit, J. H.↗

Laser furnace technology for zone refining

A carbon dioxide laser experiment facility is constructed to investigate the problems in using a laser beam to zone refine semiconductor and metal crystals. The hardware includes a computer to control scan mirrors and stepper motors to provide a variety of melt zone patterns. The equipment and its operating procedures are described.

Griner, D. B.↗

Traveling Molten Zone Refining Process Development for Innovative Fuel Cycle Solutions

Considering the phase diagrams of metallic spent fuel constituents, the melting and solidifying of spent metallic fuel causes three immiscible layers (actinide-rich, lanthanide-rich, and Group II-rich) and the condensate phase (Group I) to form. We believe this anticipated immiscibility offers an untapped opportunity for innovative fuel cycle solutions. Through the proposed project, we anticipate confirming the expected phase behavior and develop a thermal treatment process to rapidly extract actinides from spent metallic fuels. The prime apparatus for both purposes is a traveling molten zone system with induction heating. We envision that one rapid pass of the molten zone from the bottom to the top of the metallic rod incorporating species of spent metallic fuels should produce the expected immiscible layer formation and provide species partitioning data effectively and cleanly. It will also demonstrate an actinide extraction process by concentrating the impurities at the top segment of the rod and leaving the actinide species behind as the bulk rod. The successful execution of the project will demonstrate proof of concept for a transformative process path for used metal fuels in terms of economics and safeguards.

36 MATERIALS SCIENCE↗

Preparation of multistage zone-refined materials for thermochemical standards

This paper describes the steps of a two-step zone purification procedure for completed minicells filled with ultrahigh-purity succinonitrile (SCN) in which the CNS is under its own vapor pressure. The solid-liquid equilibrium, as determined by melting and freezing point measurements, is therefore considered to be a realization of the triple-point. The freezing-point plateaus measured at a variety of bath temperatures demonstrated both the fundamental reproducibility of the measurement for a given sample and the lack of dependence of that measurement on the bath temperature which controls the freezing rate. The measurement reproducibility and the sample consistency indicate that the method described is indeed suitable for the preparation of pure material which can be used for the purposes of thermistor and thermometer calibration at 58.0796 + or - 0.0015 C.

Rubinstein, E.↗

Float zone refining: Space problems and solutions. A speculative proposal

A facility for the automatic growth of 60 cm long boules of Si up to 10 cm diameter is described. The facility is 21 ft tall, weighs 17,000 lb (without the sand ballast), and consumes 60 kW power. As a point of reference, the facility will cost approximately $500K without automation which will be developed. The total price is expected to be approximately $1.2 million.

Gill, G.↗

Purification and Crystal Growth of Lead Iodide by Physical Vapor Transport Method

Lead iodide (PbI2) is a layered compound semiconductor being developed as room temperature x- and gamma-ray detector. Compared to the more studied material, mercuric iodide, PbI2 has a higher melting temperature and no phase transition until liquid phase which are indications of better mechanical properties. In this study, the source material was purified by the zone-refining process, and the purest section was extracted from center of the the zone-refined ingot to be grown by physical vapor transport (PVT) method. The zone-refined material and as-grown crystals were characterized by optical microscopy and differential scanning calorimetry (DSC) to reveal the surface morphology, purity and stoichiometry. The results shows that both materials are near-stoichiometric composition, with the purity of the as-grown crystals higher than zone-refined materials. The resistivity of the as-grown crystal (10" Omega-cm) was derived from current-voltage (I-V) measurement, and is 10 times higher than the zone-refined materials. Detail results will be presented and discussed.

Wright, G. W.↗

Purification of Carbon Nanotubes: Alternative Methods

Traditional carbon nanotube purification process involves nitric acid refluxing and cross flow filtration using surfactant TritonX. This is believed to result in damage to nanotubes and surfactant residue on nanotube surface. Alternative purification procedures involving solvent extraction, thermal zone refining and nitric acid refiuxing are used in the current study. The effect of duration and type of solvent to dissolve impurities including fullerenes and P ACs (polyaromatic compounds) are monitored by nuclear magnetic reasonance, high performance liquid chromatography, and thermogravimetric analysis. Thermal zone refining yielded sample areas rich in nanotubes as seen by scanning electric microscopy. Refluxing in boiling nitric acid seem to improve the nanotube content. Different procedural steps are needed to purify samples produced by laser process compared to arc process. These alternative methods of nanotube purification will be presented along with results from supporting analytical techniques.

Files, Bradley↗

Succinonitrile Purification Facility

The Succinonitrile (SCN) Purification Facility provides succinonitrile and succinonitrile alloys to several NRA selected investigations for flight and ground research at various levels of purity. The purification process employed includes both distillation and zone refining. Once the appropriate purification process is completed, samples are characterized to determine the liquidus and/or solidus temperature, which is then related to sample purity. The lab has various methods for measuring these temperatures with accuracies in the milliKelvin to tenths of milliKelvin range. The ultra-pure SCN produced in our facility is indistinguishable from the standard material provided by NIST to well within the stated +/- 1.5mK of the NIST triple point cells. In addition to delivering material to various investigations, our current activities include process improvement, characterization of impurities and triple point cell design and development. The purification process is being evaluated for each of the four vendors to determine the efficacy of each purification step. We are also collecting samples of the remainder from distillation and zone refining for analysis of the constituent impurities. The large triple point cells developed will contain SCN with a melting point of 58.0642 C +/- 1.5mK for use as a calibration standard for Standard Platinum Resistance Thermometers (SPRTs).

Source record↗

Elucidating microstructural evolution and hardness variation across friction self-piercing riveted Al-7055 using synchrotron X-ray scattering and advanced microscopy techniques

Friction self-piercing riveting (FSPR) is a unique hybrid joining technique that combines the advantages of mechanical interlocking, frictional heat, and solid-state joining (if metallurgically compatible) to produce crack free joints in high strength and/or low-ductility alloys at room temperature. Here, in the current study, Al-7055 sheets were joined using FSPR for lightweight automotive applications and significant microhardness variations were observed across the joint cross-section. A detailed microstructural characterization at multiple length scales was carried out using advanced electron microscopy and X-ray scattering techniques to provide a fundamental understanding of the process-structure-property relationships. The relative contributions of microstructural characteristics at various length scales (i.e., grain size, dislocation density, solute concentration, precipitate nature) to strengthening were estimated using existent formulations (i.e., Hall-Petch, Taylor, precipitate bypass/shear equations) and correlated to the observed microhardness values across different regions. Small-angle X-ray scattering and scanning transmission electron microscopy revealed significant changes in the size and volume fraction of precipitate species, i.e., GP-I Zones, η′, and Mg/Zn solute co-clusters, depending on the process region. It was observed that the dissolution of the small η′/GP-I zones (T ∼ 150–200 °C) in the heat-affected zone were the key reason for the hardness drop. Further, it was shown that solid-solution, dislocation, grain size and solute co-cluster strengthening played a key role in the thermo-mechanically affected zone and grain-refined zone (GRZ). Finally, these observations were leveraged along with the Zener-Holloman relationship and grain size in the GRZ to estimate the peak joining temperature of the GRZ (∼ 350 °C) near the steel rivet.

aluminum 7xxx alloy↗