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At least 73 records · Page 4

Study of factors determining the radiation sensitivity of quartz crystal oscillators (A0189)

The correlation between defect cluster concentrations observed for different grades of quartz examined by transmission electron microscopy (TEM) and the electrical stability of quartz resonators exposed to complex radiation in an orbital LDEF was determined. It is demonstrated that the technique TEM provides a powerful method for studying the effect of radiation on crystalline quartz. Two factors suggest that the observed clusters may be responsible for the radiation-induced frequency drift and acoustic absorption effects associated with irradiated quartz resonators: (1) the clusters are expected to be very effective in modifying the piezoelectric properties of quartz because of the large strain fields associated with them; (2) both phenomena appear to be sensitive to the impurity concentration. It is suggested that TEM can be used to classify grades of quartz according to their suitability for use in radiation-hard resonators. This technique may identify the impurities that are responsible and thereby effect an improvement in the stability of quartz oscillators.

Venables, J. D.↗

Thermal and sputtered aluminum oxide coatings for high temperature electrical insulation

Aluminum oxide coatings have been investigated as electrically insulating layers for mounting thin film Pt-Pt/Rh thermocouples on gas turbine blade and vane alloys (MAR M200 + Hf and MAR M509). Thermal oxides were grown directly onto NiCoCrAlY and FeCrAlY coatings on these alloys at temperature between 1300 and 1400 K in oxygen partial pressures 10 to the -7th to 2 x 10 to the 4th Pa. Although these thermal oxides exhibited good adherence, analytical characterizations using electron and optical microscopy, as well as X-ray photoelectron spectroscopy showed that they had defects and impurities which limited their insulating ability. The insulating quality of the coating was greatly improved however by reactively sputtering an aluminum oxide film over the thermal oxide. Results are presented on the electrical performance of the 2-5 micron thick composite layers for temperatures up to 1300 K.

Kreider, K. G.↗

Offset-Stoichiometric Reflowable Composite Bonding Method with Adhesive for Mitigating Strict Faying Surface Tolerances

Inherent susceptibility of adhesive bonds to miniscule quantities of contamination can cause undetectable weakened bonds. For this reason, the Federal Aviation Administration (FAA) places strict regulations on adhesively bonded joints in primary aircraft structures. To meet certification requirements aircraft manufactures resort to redundant load paths in the form of fasteners which inherently add weight to the structure and increase manufacturing time. In prior work, a secondary bonding technique called AERoBOND was developed, which utilized off-stoichiometric epoxymatrix resins to facilitate reflow and diffusion of the resin within the joint interface during a secondary bonding/cure process, thus achieving a bond similar to a co-cured joint. However, the AERoBOND process required tight spatial tolerances between the two parts being joined. This study examined the utilization of conventional adhesive with the AERoBOND method to act as a filler in the joint line, effectively reducing the need for tight tolerances on the joining parts and serving as a flexible alternative for existing manufacturing processes. Ultrasonic inspection, optical microscopy, and ASTM International standard tests were performed to analyze the joints for defects and to quantify the mode-I and mode-II interlaminar fracture toughness and short beam strength of the proposed methodology with varying manufacturing parameters. The comprehensive results indicate that the AERoBOND+ method with and without surface preparation performs comparably to co-cured and conventional, adhesively bonded joints when secondary cured in an autoclave with 791 kPa of pressure. As an example, the AERoBOND+ panel without surface preparation bonded with 791 kPa of pressure (referred to as AB+3 throughout paper) had a mode-I fracture toughness (G Ic ) of 0.643 kJ/m 2 and a mode-II fracture toughness (G IIc ) of 4.000 kJ/m 2 in the non-precracked condition and 4.218 kJ/m 2 in the precracked condition at the adhesive-to-prepreg interface. These results were 96%, 142%, and 217%, respectively, of a co-cured baseline panel (referred to as C1 throughout paper).

Composites↗

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

During the past year we have focused on application of in situ Atomic Force Microscopy (AFM) for studies of the growth mechanisms and kinetics of crystallization for different macromolecular systems. Mechanisms of macrostep formation and their decay, which are important in understanding of defect formation, were studied on the surfaces of thaumatin, catalase, canavalin and lysozyme crystals. Experiments revealed that step bunching on crystalline surfaces occurred either due to two- or three-dimensional nucleation on the terraces of vicinal slopes or as a result of uneven step generation by complex dislocation sources. No step bunching arising from interaction of individual steps in the course of the experiment was observed. The molecular structure of the growth steps for thaumatin and lipase crystals were deduced. It was further shown that growth step advance occurs by incorporation of single protein molecules. In singular directions growth steps move by one-dimensional nucleation on step edges followed by lateral growth. One-dimensional nuclei have different sizes, less then a single unit cell, varying for different directions of step movement. There is no roughness due to thermal fluctuations, and each protein molecule which incorporated into the step remained. Growth kinetics for catalase crystals was investigated over wide supersaturation ranges. Strong directional kinetic anisotropy in the tangential step growth rates in different directions was seen. The influence of impurities on growth kinetics and cessation of macromolecular crystals was studied. Thus, for catalase, in addition to pronounced impurity effects on the kinetics of crystallization, we were also able to directly observe adsorption of some impurities. At low supersaturation we repeatedly observed filaments which formed from impurity molecules sedimenting on the surfaces. Similar filaments were observed on the surfaces of thaumatin, canavalin and STMV crystals as well, but the frequency was low compared with catalase crystallization. Cessation of growth of xylanase and lysozyme crystals was also observed and appeared to be a consequence of the formation of dense impurity adsorption layers. Attachment: "An in situ AFM investigation of catalase crystallization", "Atomic force microscopy studies of living cells: visualization of motility, division, aggregation, transformation, and apoptosis", AFM studies on mechanisms of nucleation and growth of macromolecular crystals", and "In situ atomic force microscopy studies of surface morphology, growth kinetics, defect structure and dissolution in macromolecular crystallization".

Malkin, Alexander J.↗

Organometallic chemical vapor deposition and characterization of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates

The epitaxial growth of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates by open tube organometallic chemical vapor deposition (OMCVD) is reported. The chemical composition of the alloys characterized by energy dispersive X-ray spectroscopy shows that alloys with x up to 0.13 can be deposited on (001) GaP. Epitaxial growth with mirror smooth surface morphology was achieved for x less than or equal to 0.05. Transmission electron microscopy (TEM) micrographs of these alloys show specular epitaxy and the absence of microstructural defects indicating a defect density of less than 10(exp 7) cm(sup -2). Selected area electron diffraction pattern of the alloy shows that the epitaxial layer crystallizes in the chalcopyrite structure with relatively weak superlattice reflections indicating certain degree of randomness in the cation sublattice. Hall measurements show that the alloys are p-type, like the unalloyed films; the carrier concentration, however, dropped about 10 times from 2 x 10(exp 18) to 2 x 10(exp 17) cm(sup -3). Absorption measurements indicate that the band tailing in the absorption spectra of the alloy was shifted about 0.04 eV towards shorter wavelength as compared to the unalloyed material. Diodes fabricated from the n(+)-GaP/p-ZnSiP2-ZnGeP2-Ge heterostructure at x = 0.05 have a reverse break-down voltage of -10.8 V and a reverse saturation current density of approximately 6 x 10(exp -8) A/sq cm.

Xing, G. C.↗

Differences in elasticity of vinculin-deficient F9 cells measured by magnetometry and atomic force microscopy

We have investigated a mouse F9 embryonic carcinoma cell line, in which both vinculin genes were inactivated by homologous recombination, that exhibits defective adhesion and spreading [Coll et al. (1995) Proc. Natl. Acad. Sci. USA 92, 9161-9165]. Using a magnetometer and RGD-coated magnetic microbeads, we measured the local effect of loss and replacement of vinculin on mechanical force transfer across integrins. Vinculin-deficient F9Vin(-/-) cells showed a 21% difference in relative stiffness compared to wild-type cells. This was restored to near wild-type levels after transfection and constitutive expression of increasing amounts of vinculin into F9Vin(-/-) cells. In contrast, the transfection of vinculin constructs deficient in amino acids 1-288 (containing the talin- and alpha-actinin-binding site) or substituting tyrosine for phenylalanine (phosphorylation site, amino acid 822) in F9Vin(-/-) cells resulted in partial restoration of stiffness. Using atomic force microscopy to map the relative elasticity of entire F9 cells by 128 x 128 (n = 16,384) force scans, we observed a correlation with magnetometer measurements. These findings suggest that vinculin may promote cell adhesions and spreading by stabilizing focal adhesions and transferring mechanical stresses that drive cytoskeletal remodeling, thereby affecting the elastic properties of the cell.

Non-NASA Center↗

Analysis of defect structure in silicon. Characterization of samples from UCP ingot 5848-13C

Statistically significant quantitative structural imperfection measurements were made on samples from ubiquitous crystalline process (UCP) Ingot 5848 - 13 C. Important trends were noticed between the measured data, cell efficiency, and diffusion length. Grain boundary substructure appears to have an important effect on the conversion efficiency of solar cells from Semix material. Quantitative microscopy measurements give statistically significant information compared to other microanalytical techniques. A surface preparation technique to obtain proper contrast of structural defects suitable for QTM analysis was perfected.

Natesh, R.↗

Ballistic-Electron-Emission Microscopy Techniques for Nanometer-scale Characterization of Interfaces

Semiconductor interface properties are among the most important phenomena in materials science and technology. The study of metal/semiconductor Schottky barrier interfaces has been the primary focus of a large research and development community for decades. Throughout the long history of interface investigation, the study of interface defect electronic properties have been seriously hindered by the fundamental experimental difficulty of probing subsurface structures. A new method, Ballistic-Electron-Emission Microscopy (BEEM), has been developed which not only enables spectroscopic probing of subsurface interface properties, but also, provides nanometer-resolution imaging capabilities. BEEM employs Scanning Tunneling Microscopy (STM) and a unique spatially localized ballistic electron spectroscopy method...

Bell, L. D.↗

Complex Intergrowths of Non-Stoichiometric Defect-Structured Hibonite and Al-Rich Spinel in an Allende Ca-Al-Rich Inclusion

Hibonite is a primary ultra-refractory mineral occurring in many Ca-Al-rich inclusions (CAIs) and is predicted to condense as the second major phase from a cooling gas of solar composition. Our previous microstructural studies of hibonite in carbonaceous chondrites revealed its unique microstructures consisting of numerous defects that contain Mg-enriched, wider spinel blocks in stoichiometric hibonite. Han, J. et al. [2 items] demonstrated experimentally that defect-structured hibonites can grow easily in the presence of minor Mg and are kinetically more stable than equilibrium assemblages predicted by thermodynamic calculations. However, a thermo-dynamic vs. structural stability of defect-structured hibonite relative to other early-condensed Al-rich phases such as corundum, grossite, and spinel remains poorly constrained. Here, we present the results of atomic resolution TEM (Transmission Electron Microscopy) imaging of hibonite in a compact Type A CAI in the Allende CV3 chondrite in order to better understand the crystal structure and chemistry of defect-structured hibonite and its associated Al-rich phases, especially non-stoichiometric, Al-rich spinel, in the context of the formation of first refractory solids in the early solar nebula.

Han, J.↗

The Mechanical Properties of a Ni-30Al-20Fe-0.05Zr Intermetallic Alloy in the Temperature Range 300-1200 K

Tensile tests were conducted on an extruded Ni-30(at. pct)Al-20Fe-0.05Zr intermetallic alloy in the temperature range 300-1200 K, and the microstructures were characterized by optical, scanning, and transmission electron microscopy. The alloy did not exhibit any room temperature ductility and failed by transgranular cleavage at a stress of about 710 MPa. This mode of fracture was observed at and below 873 K with the total ductility being less than 2.5 percent. However, the failure mode changed to dimpled fracture, triple point cracking, and rupture above 873 K. Scanning electron microscopy of the fracture surfaces revealed that transgranular cleavage failure had always originated at preexisting defects. In these cases, the fracture stress exhibited a good correlation with the defect size, in accordance with linear elastic fracture mechanics, where the critical stress intensity factor was estimated to be about 4 MPa sq rt m.

Raj, S. V.↗

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Kim, Hyun Jung↗

Defect characterization of silicon dendritic web ribbons

Progress made in the study of defect characterization of silicon dendritic web ribbon is presented. Chemical etching is used combined with optical microscopy, as well as the electron beam induced current (EBIC) technique. Thermal annealing effect on carrier lifetime is examined.

Cheng, L. J.↗

A Screening Method Using Pulsed-Power Combined with Infrared Imaging to Detect Pattern Defects in Bulk Metal Foil or Thin Film Resistors

Bulk metal foil and thin film resistors occasionally contain localized defects within the etched resistor pattern. Common defects of this type include in-line constrictions referred to as notches, unremoved resistor material bridges between adjacent pattern lines, and embedded non-conductive particles in the resistor material. Such defects are prone to fracture due to thermomechanical fatigue during powered operation, especially power cycling, resulting in positive resistance change and open circuit failure modes. Common screening methods of optical microscopy, short time overload power tests (e.g., 6.25x rated power for 5 seconds) and burn-in (e.g., 1.5x rated power for 100 hours) are useful, but they are not always effective at removing devices with such defects. An improved method has been developed to screen for localized resistor pattern defects. The method involves the application of brief, high power electrical pulses at a low duty cycle while inspecting the resistor with a high resolution, high speed infrared camera. The following test conditions were found to be suitable for this purpose: 6.25x rated power, 1 to 5 pulses, 50 ms pulse width and 10% duty cycle. During the power pulsing, localized constrictions in the resistor pattern are identifiable as hot spots via the infrared camera. Reject criteria can be established based on observations of hot spots. To assess its effectiveness, a total of two hundred eighty (280) surface mount foil resistors (40 each from 7 different lots) were screened using this infrared technique. The screening identified twenty-nine (29) resistors with significant hot spots in the resistor pattern. All 280 resistors were then subjected to an industry standard 10,000 hour life test at 1x rated power at 70°C with power cycled for 90 minutes on and 30 minutes off. During life testing, three resistors exhibited positive resistance change failure mode. All three failures were due to thermomechanical fatigue failure of localized bridge defects at the locations identified via infrared screening. The results of this evaluation illustrate the benefits of the pulsed-power infrared detection screening technique to identify reliability suspect foil or thin film resistors that may escape common screening methods.

screening↗

A Screening Method Using Pulsed-Power Combined with Infrared Imaging to Detect Pattern Defects in Bulk Metal Foil or Thin Film Resistors

Bulk metal foil and thin film resistors occasionally contain localized defects within the etched resistor pattern. Common defects of this type include in-line constrictions referred to as notches, unremoved resistor material bridges between adjacent pattern lines, and embedded non-conductive particles in the resistor material. Such defects are prone to fracture due to thermomechanical fatigue during powered operation, especially power cycling, resulting in positive resistance change and open circuit failure modes. Common screening methods of optical microscopy, short time overload power tests (e.g., 6.25x rated power for 5 seconds) and burn-in (e.g., 1.5x rated power for 100 hours) are useful, but they are not always effective at removing devices with such defects. An improved method has been developed to screen for localized resistor pattern defects. The method involves the application of brief, high power electrical pulses at a low duty cycle while inspecting the resistor with a high resolution, high speed infrared camera. The following test conditions were found to be suitable for this purpose: 6.25x rated power, 1 to 5 pulses, 50 ms pulse width and 10% duty cycle. During the power pulsing, localized constrictions in the resistor pattern are identifiable as hot spots via the infrared camera. Reject criteria can be established based on observations of hot spots. To assess its effectiveness, a total of two hundred eighty (280) surface mount foil resistors (40 each from 7 different lots) were screened using this infrared technique. The screening identified twenty-nine (29) resistors with significant hot spots in the resistor pattern. All 280 resistors were then subjected to an industry standard 10,000 hour life test at 1x rated power at 70°C with power cycled for 90 minutes on and 30 minutes off. During life testing, three resistors exhibited positive resistance change failure mode. All three failures were due to thermomechanical fatigue failure of localized bridge defects at the locations identified via infrared screening. The results of this evaluation illustrate the benefits of the pulsed-power infrared detection screening technique to identify reliability suspect foil or thin film resistors that may escape common screening methods.

screening↗

Superconductivity in the high-Tc Bi-Ca-Sr-Cu-O system - Phase identification

Four phases are observed in superconducting Bi-Ca-Sr-Cu-O samples. The superconducting phase, with onset temperature near 120 K, is a 15.4-A-layered compound with composition near Bi2Ca1Sr2Cu2O9 and an A-centered orthorhombic unit subcell 5.41 x 5.44 x 30.78 A. X-ray diffraction and electron microscopy data are consistent with a structure of alternating perovskite and Bi2O2 layers. High-resolution transmission electron microscopy images reveal a b-axis superstructure of 27.2 A, numerous (001) stacking faults, and other defects.

Hazen, R. M.↗

Quantification Of 4H- To 3C-Polymorphism In Silicon Carbide (SiC) Epilayers And An Investigation Of Recombination-Enhanced Dislocation Motion In SiC By Optical Emission Microscopy (Oem) Techniques

Environments that impose operational constraints on conventional silicon-(Si) based semiconductor devices frequently appear in military- and space-grade applications. These constraints include high temperature, high power, and high radiation environments. Silicon carbide (SiC), an alternative type of semiconductor material, has received abundant research attention in the past few years, owing to its radiation-hardened properties as well as its capability to withstand high temperatures and power levels. However, the growth and manufacture of SiC devices is still comparatively immature, and there are severe limitations in present crystal growth and device fabrication processes. Among these limitations is a variety of crystal imperfections known as defects. These imperfections can be point defects (e.g., vacancies and interstitials), line defects (e.g., edge and screw dislocations), or planar defects (e.g., stacking faults and double-positioning boundaries). All of these defects have been experimentally shown to be detrimental to the performance of electron devices made from SiC. As such, it is imperative that these defects are significantly reduced in order for SiC devices to become a viable entity in the electronics world. The NASA Glenn High Temperature Integrated Electronics & Sensors Team (HTIES) is working to identify and eliminate these defects in SiC by implementing improved epitaxial crystal growth procedures. HTIES takes two-inch SiC wafers and etches patterns, producing thousands of mesas into each wafer. Crystal growth is then carried out on top of these mesas in an effort to produce films of improved quality-resulting in electron devices that demonstrate superior performance-as well as fabrication processes that are cost-effective, reliable, and reproducible. In this work, further steps are taken to automate HTIES' SiC wafer inspection system. National Instruments LabVIEW image processing and pattern recognition routines are developed that are capable of quantifying and mapping defects on both the substrate and mesa surfaces, and of quantifying polymorphic changes in the grown materials. In addition, an optical emission microscopy (OEM) system is developed that will facilitate comprehensive study of recombination-enhanced dislocation motion (REDM).

Speer, Kevin M.↗

Silicon Carbide Epitaxial Films Studied by Atomic Force Microscopy

Silicon carbide (SiC) holds great potential as an electronic material because of its wide band gap energy, high breakdown electric field, thermal stability, and resistance to radiation damage. Possible aerospace applications of high-temperature, high-power, or high-radiation SiC electronic devices include sensors, control electronics, and power electronics that can operate at temperatures up to 600 C and beyond. Commercially available SiC devices now include blue light-emitting diodes (LED's) and high-voltage diodes for operation up to 350 C, with other devices under development. At present, morphological defects in epitaxially grown SiC films limit their use in device applications. Research geared toward reducing the number of structural inhomogeneities can benefit from an understanding of the type and nature of problems that cause defects. The Atomic Force Microscope (AFM) has proven to be a useful tool in characterizing defects present on the surface of SiC epitaxial films. The in-house High-Temperature Integrated Electronics and Sensors (HTIES) Program at the NASA Lewis Research Center not only extended the dopant concentration range achievable in epitaxial SiC films, but it reduced the concentration of some types of defects. Advanced structural characterization using the AFM was warranted to identify the type and structure of the remaining film defects and morphological inhomogeneities. The AFM can give quantitative information on surface topography down to molecular scales. Acquired, in part, in support of the Advanced High Temperature Engine Materials Technology Program (HITEMP), the AFM had been used previously to detect partial fiber debonding in composite material cross sections. Atomic force microscopy examination of epitaxial SiC film surfaces revealed molecular-scale details of some unwanted surface features. Growth pits propagating from defects in the substrate, and hillocks due, presumably, to existing screw dislocations in the substrates, were imaged. Away from local defects, step bunching was observed to yield step heights of hundreds of angstroms, with possible implications for the uniformity of dopants incorporated in SiC devices during fabrication. The quantitative topographic data from the AFM allow the relevant defect information to be extracted, such as the size and distribution of step bunching and the Burgers vector of screw dislocations. These atomic force microscopy results have furthered the understanding of the dynamic epitaxial SiC growth process. A model describing the observed hillock step bunching has been proposed. This cooperation between researchers involved in crystal growth, electronic device fabrication, and surface structural characterization is likely to continue as atomic force microscopy is used to improve SiC films for high-temperature electronic devices for NASA's advanced turbine engines and space power devices, as well as for future applications in the automotive industry.

Source record↗

The metal to metal interface and its effect on adhesion and friction

The paper considers the interface between two bulk metals and the effect of this interface on adhesive bonding, resistance to tangential displacements, friction and the interfacial transport from one surface to another. Using Auger emission spectroscopy, field ion microscopy, and low energy electron diffraction techniques, the influence of surface orientation, lattice registry, crystal lattice structure and defects, metal surface chemistry and alloying on the characteristics of the interface was studied for noble, platinum, transition, and Group 4B metals. With dissimilar metals in contact, epitaxial transfer of the cohesively weaker to the cohesively stronger metal has been observed. Surface chemical activity of the noble and platinum metals is shown to affect interfacial behavior as does a valence bonding in the transition metals, and the degree of metallic nature in the Group 4B elements. Alloying elements, e.g., Si and Fe, can alter interfacial behavior by segregation to the surface of metals or by altering bulk properties such as crystal transformation kinetics.

Buckley, D. H.↗