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Quantitative Analysis of Defects in Silicon

The evaluation and prediction of the conversion efficiency for a variety of silicon samples with differences in structural defects, such as grain boundaries, twin boundaries, precipitate particles, dislocations, etc. are discussed. Quantitative characterization of these structural defects, which were revealed by etching the surface of silicon samples, is performed by using an image analyzer. Due to different crystal growth and fabrication techniques the various types of silicon contain a variety of trace impurity elements and structural defects. The two most important criteria in evaluating the various silicon types for solar cell applications are cost and conversion efficiency.

Natesh, R.↗

Large-area silicon sheet task

A set of computer models was used to define a growth system configuration that was then built and used to grow web with lower thermally generated stress. Aspects of research in the edge-defined film-fed growth (EFG) method of making Si ribbon are reported. A technique was developed to determine base resistivity and carrier lifetime in semicrystalline wafers. Automated growth of 150 kg of 15 cm-dia ingot material per crucible is reviewed. Scanning transmisson electron microscopy (STEM) and microprobe investigations of processed EFG ribbon are reported. The chemical composition of the large precipitates was studied. The structural arrangement and the electrical activity of distentions or close to the central twin plane in processed material were studied. The electrical and structural properties of grain boundaries in silicon are discussed. Temperature-dependence measurements of zero-bias conductance, a photoconductivity technique, and deep-level transient spectroscopy (DLTS) were developed. A grooving and staining technique, secondary ion mass spectroscopy, and EBIC measurements in scanning electron microscopy were used to study enhanced diffusion of phosphorus at grain boundaries in polycrystaline silicon. The fundamental mechanisms of abrasion and wear and the deformation of Si by a diamond in various fluid environments are described. The efficiency of solar cells made from EFG ribbon and Semix Inc. material is reported.

Morrison, A. D.↗

Literature survey on oxidations and fatigue lives at elevated temperatures

Nickel-base superalloys are the most complex and the most widely used for high temperature applications such as aircraft engine components. The desirable properties of nickel-base superalloys at high temperatures are tensile strength, thermomechanical fatigue resistance, low thermal expansion, as well as oxidation resistance. At elevated temperature, fatigue cracks are often initiated by grain boundary oxidation, and fatigue cracks often propagate along grain boundaries, where the oxidation rate is higher. Oxidation takes place at the interface between metal and gas. Properties of the metal substrate, the gaseous environment, as well as the oxides formed all interact to make the oxidation behavior of nickel-base superalloys extremely complicated. The important topics include general oxidation, selective oxidation, internal oxidation, grain boundary oxidation, multilayer oxide structure, accelerated oxidation under stress, stress-generation during oxidation, composition and substrate microstructural changes due to prolonged oxidation, fatigue crack initiation at oxidized grain boundaries and the oxidation accelerated fatigue crack propagation along grain boundaries.

Liu, H. W.↗

Grain Boundary Engineering the Mechanical Properties of Allvac 718Plus(Trademark) Superalloy

Grain Boundary Engineering can enhance the population of structurally-ordered "low S" Coincidence Site Lattice (CSL) grain boundaries in the microstructure. In some alloys, these "special" grain boundaries have been reported to improve overall resistance to corrosion, oxidation, and creep resistance. Such improvements could be quite beneficial for superalloys, especially in conditions which encourage damage and cracking at grain boundaries. Therefore, the effects of GBE processing on high-temperature mechanical properties of the cast and wrought superalloy Allvac 718Plus (Allvac ATI) were screened. Bar sections were subjected to varied GBE processing, and then consistently heat treated, machined, and tested at 650 C. Creep, tensile stress relaxation, and dwell fatigue crack growth tests were performed. The influences of GBE processing on microstructure, mechanical properties, and associated failure modes are discussed.

Gabb, Timothy P.↗

Defects in High Speed Growth of EFG Silicon Ribbon

Silicon ribbons grown by the Edge-defined Film-fed Growth (EFG) technique exhibit a characteristic defect structure typified by twins, dislocations, grain boundaries and silicon carbide inclusions. As growth speed is increased from less than 2.5 cm per minute, the structural details change. The major difference between the ribbons grown at speeds below and above 2.5 cm per minute is in the generation of a cellular structure at the higher growth speeds, observable in the ribbon cross section. The presence of the cross sectional structure leads, in general, to a reduction in cell performance. Models to explain the formation of such a cross sectional structure are presented and discussed.

Rao, C. V. H. N.↗

Design principles for high efficiency small-grain polysilicon solar cells, with supporting experimental studies

Design principles suggested here aim toward high conversion efficiency (greater than 15 percent) in polysilicon cells. The principles seek to decrease the liabilities of both intragranular and grain-boundary-surface defects. The advantages of a phosphorus atom concentration gradient in a thin (less than 50 microns) base of a p(+)/n(x)/n(+) drift-field solar cell, which produces favorable gradients in chemical potential, minority-carrier mobility and diffusivity, and recombination lifetime (via phosphorus gettering) are suggested. The degrading effects of grain boundaries are reduced by these three gradients and by substituting atoms (P, H, F or Li) for vacancies on the grain-boundary surface. From recent experiments comes support for the benefits of P diffusion down grain boundaries and, for quasi-grain-boundary-free and related structures. New analytic solutions for the n(x)-base include the effect of a power-law dependence between P concentration and lifetime. These provide an upper-bound estimate on the open circuit voltage. Finite-difference numerical solutions of the six Shockley equations furnish complete information about all solar-cell parameters and add insight concerning design.

Lindholm, F. A.↗

The influence of isothermal annealing on the molybdenum fibers of a directed solid gamma/gamma prime - alpha alloy

The mechanical characteristics of the directed solid eutectic Ni-Al-Mo (gamma/gamma prime)-alpha alloy at high temperatures make it useful in the blades of gas turbines. Structural changes are observed for the alloy under isothermal annealing, particularly the formation of molybdenum plates at the grain boundary and an increase of the gamma phase in relation to the gamma prime phase. Molybdenum lamellas appear at the grain boundary above 1100 C which can have a negative influence on the mechanical properties. The change in the structure near the grain boundary with the increase in temperature is illustrated through a sequence of pictures.

Whittenberger, J. D.↗

Effects of cobalt, boron, and zirconium on the microstructure of Udimet 738

A structural study was carried out on Co modified Udimet 738 alloys containing 0.04, 0.10, and 0.20 wt % Zr at 0.01 and 0.03 wt % B levels. Samples in the as-cast and solution-treated conditions were exposed at 843 C to study structural stability. The structures produced by the interactions of Co, Zr, and B were studied by SEM, X-ray diffraction, and dispersive analysis techniques. The additions of large amounts of Zr and B were found to increase the solidification range of the U-738. Structural changes involved eutectic gamma prime islands, formation of low melting point compounds, and precipitation of borides and Zr rich phases. Boron and zirconium additions did not show substantial changes in mechanical properties. Removal of Co from the alloys resulted in reduction of the matrix solubility for carbon and increase in the gamma prime solvus. Structural instabilities found were continuous grain boundary M23C6 films, MC breakdown, and plate-like phases. Removal of cobalt resulted in a slight decrease in tensile and stress rupture properties. Detailed structural results presented.

Nakanishi, T. G.↗

TPSAS-NF1676L-13792-DND

Extreme structural requirements of future aerospace vehicles motivate the development of new, ultra-durable materials and game-changing methodologies for material certification and sustainment. Computational simulations spanning many orders of magnitude in length and time scales—from the nanoscale of underlying damage processes to the larger scales of continuum cracks—are being developed to support these requirements. Results of these simulations are used to deduce key aspects of material response to loads and environments, including: - The microstructural mechanics that govern metal fatigue crack initiation and growth - The variety and complexity of the dislocation-precipitate interac- tions that underpin plastic behavior and damage evolution - The energetic principles that govern the interaction of water with crack surfaces within a structural component - The mechanics of grain boundary separation Modeling the physics behind these metal fatigue behaviors is extremely complex, and requires intensive, high-fidelity simulations. The knowledge gained through these simulations, however, is forming the keystone for advanced material design and will enable development of more capable, reliable structures for aerospace vehicles.

Jacob Hochhalter↗

Hydrogen trapping and the interaction of hydrogen with metals

A method has been developed for the determination of trapped hydrogen in metal alloys, involving the determination of mobile hydrogen using the electrochemical method and the determination of total hydrogen with the fusion method, the difference in hydrogen concentrations being due to trapped hydrogen. It has been found that hydrogen enters body-centered cubic structures through the grain bodies rather than through the grain boundaries. Hydrogen also diffuses much more rapidly in body-centered cubic structures on charging than in face-centered cubic structures, the hydrogen distribution being more uniform in nature. The energy necessary to cause hydrogen embrittlement is postulated to arise from the changes in crystal lattice energies brought about through interaction of hydrogen with atoms in the metal lattice. The total energy change is more negative for body-centered cubic structures, believed to be the cause of a greater tendency toward hydrogen embrittlement. Finally, the agreement of hydrogen concentrations obtained at 25 C by the electrochemical method with those obtained by the fusion method are taken as a strong indication of the power and validity of the electrochemical method.

Danford, Merlin D.↗

Ultrahigh Temperature Ceramics for Thermal Protection of Next Generation Space Vehicles

Materials with improved properties are needed for thermal protection of next generation space vehicles. Sharp leading edges on these vehicles will have to withstand exposure to high temperatures (> 2200 C or 4000 F) and severe thermal cycling in both neutral and oxidizing environments. These extreme conditions will require materials that possess superior oxidation resistance, low creep, and excellent thermal shock properties. This presentation will first discuss the system requirements for thermal protection of advanced space vehicles and then show how they are driving development of new materials systems. The presentation will focus on ultrahigh temperature ceramics (UHTCs) that are promising candidates for such applications. ZrB2 and HfB2 and composites of those ceramics with SiC are two particular families of UHTCs that are currently under development for sharp leading edges. These ceramics are appealing because their melting temperatures are 3245 C (5873 F) for ZrB2 and 3380 C (6116 F) for HfB2 and because they may form protective, oxidation resistant coatings in use. The mechanical properties of the UHTCs are strongly dependent on phase purity and the processing route used to make them, both of which factors are being actively investigated. For example, oxide impurities could form glassy grain boundary phases that soften at high temperatures and make the ceramic susceptible to creep deformation. Results from scanning and transmission electron microscopic studies of the UHTCs have shown how their processing can be improved to give better properties. This presentation will discuss the UHTC characterization results in some detail, focusing particularly on the structure and composition of the ceramic grain boundaries. The presentation will conclude with some remarks on how the properties of these promising UHTCs can be further improved and how they might be made more economically.

Loehman, R. E.↗

A Compendium of Scale Surface Microstructures: Ni(pt)al Coatings Oxidized at 1150 C for 2000 1-h Cycles

The surface structure of scales formed on Ni(Pt)Al coatings was characterized by SEM/EDS/BSE in plan view. Two nominally identical {100} samples of aluminide coated CMSX4 single crystal were oxidized at 1150 C for 2000 1-h cycles and were found to produce somewhat disparate behavior. One sample, with less propensity for coating grain boundary ridge deformation, presented primarily alpha-Al2O3 scale structures, with minimal weight loss and spallation. The original scale structure, still retained over most of the sample, consisted of the classic theta-alpha transformation-induced ridge network structure, with approx. 25 nm crystallographic steps and terraces indicative of surface rearrangement to low energy alumina planes. The scale grain boundary ridges were often decorated with a fine, uniform distribution of (Hf,Ti)O2 particles. Another sample, producing steady state weight losses, exhibited much interfacial spallation and a complex assortment of different structures. Broad areas of interfacial spalling, crystallographically-faceted (Ni,Co)(Al,Cr)2O4 spinel, with an alpha-Al2O3 base scale, were the dominant features. Other regions exhibited nodular spinel grains, with fine or (Ta,Ti)-rich (rutile) particles decorating or interspersed with the spinel. While these features were consistent with a coating that presented more deformation at extruded grain boundaries, the root cause of the different behavior between the duplicate samples could not be conclusively identified.

Smialek, James L.↗

Relaxation behavior of ultrasonic attenuation in YBa2Cu3O7

It is shown that temperature-dependent ultrasonic attenuation data of YBa2Cu3O7 at various frequencies exhibit anomalies at temperatures close to Tc. These attenuation maxima are found to be the result of a relaxation mechanism added on top of an unusual attenuation background. It is proposed that the grain boundary motions induced by the structural distortion and the propagation of sound waves enhances the energy dissipation around Tc. Whether this structural distortion is the consequence of the onset of a superconducting state remains undetermined. It is also possible that either a tunneling effect or the acoustoelectric effect contributes to sound energy dissipation. The temperature dependence of ultrasonic velocity shows a softening around Tc which may be an intrinsic property of high-temperature superconductors.

Sun, K. J.↗

Pinning, flow and plastic deformation of flux vortices in high T(sub c) superconductors

In high temperature superconductor (HTSC) materials the vortices are highly mobile and flexible. This is reflected in different models of melt of a vortex lattice. Another aspect of the problem is stressed: an easy nucleation and high mobility of dislocations in the vortex lattice. Some models of plastic deformation of vortex lattice are considered as a result of its interaction with a real crystal structure. Depinning is interpreted as yield of plastic flow is vortex medium. Effect of macroscopic defects in crystal structures (pores, inclusions, grain and domain boundaries) is being considered in detail. Available experimental facts on magnetization and a critical current in HTSC and conventional superconductors are discussed from the points of view of depinning to vortices vs. plastic flow of vortices vs. plastic flow of vortices medium.

Roytburd, A.↗

Superior Tensile Creep Behavior of A Novel Oxide Dispersion Strengthened Crconi Multi-Principal Element Alloy

The creep behavior of an additively manufactured (AM) yttrium oxide dispersion strengthened (ODS) CrCoNi multi-principal element alloy (MPEA) is investigated in this study. Tests were conducted over a constant tensile stress range of 40–200 MPa and a temperature range of 973–1173 K. A stress exponent of 6.5 ± 0.1 and activation energies in the range of 335–367 kJ/mol were measured. Compared to its non-ODS counterpart and its parent alloy (CrMnFeCoNi), AM ODS CrCoNi has superior creep resistance at all tested stresses and temperatures. The mechanism contributing to the excellent creep resistance of AM ODS CrCoNi is attributed to the interaction of mixed character dislocations with oxide particles. The creep ductility of AM ODS CrCoNi is higher than its nonODS counterpart due to a large percentage of low angle grain boundaries associated with its columnar grain structure. It was also found that creep ductility is significantly greater at the highest applied stress of 200 MPa compared to lower stresses. The steady state dislocation structure of AM ODS CrCoNi consists of long arrays of dislocations, which is different from that observed in non-ODS CrCoNi which consists of individual curved dislocations.

Seyed Gianmarco Sahragard-Monfared↗

TEM observations on grain boundaries in sintered silicon, part 1

Grain boundaries in silicon with a predetermined orientation were prepared by the sintering of two single crystals. A combination of standard transmission electron microscopy and lattice imaging was used to investigate the structure of the boundaries produced. Low angle grain boundaries on (100) and (111) planes, and twin boundaries on (111) planes are discussed in detail.

Ast, D. G.↗

TEM and SEM (EBIC) investigations of silicon bicrystals

The electrical and structural properties of low and medium angle tilt grain boundaries in silicon bicrystals were studied in order to obtain insight into the mechanisms determining the recombination activity. The electrical behavior of these grain boundaries was studied with the EBIC technique. Schottky barriers rather than p-n junctions were used to avoid annealing induced changes of the structure and impurity content of the as-grown crystals. Transmission electron spectroscopy reveals that the 20 deg boundary is straight, homogeneous, and free of extrinsic dislocations. It is concluded that, in the samples studied, the electrical effect of grain boundaries appears to be independent of the boundary misorientation. The dominant influence appears to be impurity segregation effects to the boundary. Cleaner bicrystals are required to study intrinsic differences in the electrical activity of the two boundaries.

Gleichmann, R.↗

Dynamic recrystallization and grain boundary migration in B2 FeAl

Transmission electron microscopy and optical microscopy were used to examine polycrystalline specimens of the B2-structured alloy FeAl strained under tension to fracture at elevated temperature. Strain-induced grain boundary migration was observed above 900 K and dynamic recrystallization was found at 1000 K and 1100 K. Little evidence of dynamic recovery was evident but some networks were formed at 1100 K.

Baker, I.↗