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Characterization of defect growth structure in ion plated films by scanning electron microscopy

Copper and gold films (0.2 to 2 microns) were ion plated onto polished 304-stainless-steel surfaces. These coatings were examined by scanning electron microscopy for coating growth defects. Three types of defects were distinguished: nodular growth, abnormal or runaway growth, and spits. The cause and origin for each type of defect was traced. Nodular growth is primarily due to inherent substrate microdefects, abnormal or runaway growth is due to external surface inclusions, and spits are due to nonuniform evaporation. All these defects have adverse effects on the coatings. They induce stresses and produce porosity in the coatings and thus weaken their mechanical properties. Friction and wear characteristics are affected by coating defects, since the large nodules are pulled out and additional wear debris is generated.

Spalvins, T.

NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

Baker, John

Histological preparation of developing vestibular otoconia for scanning electron microscopy

The unique nature of vestibular otoconia as calcium carbonate biominerals makes them particularly susceptible to chemical deformation during histological processing. We fixed and stored otoconia from all three otolith endorgans of embryonic, hatchling and adult Japanese quail in glutaraldehyde containing either phosphate or non-phosphate buffers for varying lengths of time and processed them for scanning electron microscopy. Otoconia from all age groups and otolith endorgans processed in 0.1 M phosphate buffer (pH 7.4) showed abnormal surface morphology when compared to acetone fixed controls. Otoconia processed in 0.1 M sodium cacodylate or HEPES buffered artificial endolymph (pH 7.4) showed normal morphology that was similar to controls. The degree of otoconial deformation was directly related to the time exposed to phosphate buffer. Short duration exposure produced particulate deformations while longer exposures resulted in fused otoconia that formed solid sheets. Otoconial surface deformation and fusing was independent of the glutaraldehyde component of the histological processing. These findings should help vestibular researchers to develop appropriate histological processing protocols in future studies of otoconia.

Non-NASA Center

Measurement of dihedral angles by scanning electron microscopy.

The extension of Hoover's (1971) technique to the case of dihedral-angle measurement is described. Dihedral angles are often determined by interferometry on thermally grooved grain boundaries to obtain information on relative interfacial energies. In the technique considered the measured angles approach the true angles as the tilt angle approaches 90 deg. It is pointed out that the scanning electron microscopy method provides a means of seeing the real root of a groove at a lateral magnification which is higher than that obtainable with interferometry.

Achutaramayya, G.

Scanning electron microscopy of a pink inclusion from the Allende meteorite

A scanning electron microscope study of a fine-grained, pin, Ca-rich inclusion from the Allende meteorite has revealed strong evidence for direct condensation of its constituent minerals from a vapor. This observation extends to the alkali-bearing phases in addition to the Ca-, Al-silicates and suggests that the feldspathoids as well as the refractory silicates are solar nebular condensates.

Grossman, L.

Scanning-electron-microscopy observations and mechanical characteristics of ion-beam-sputtered surgical implant alloys

An electron bombardment ion thruster was used as an ion source to sputter the surfaces of orthopedic prosthetic metals. Scanning electron microscopy photomicrographs were made of each ion beam textured surface. The effect of ion texturing an implant surface on its bond to bone cement was investigated. A Co-Cr-W alloy and surgical stainless steel were used as representative hard tissue implant materials to determine effects of ion texturing on bulk mechanical properties. Work was done to determine the effect of substrate temperature on the development of an ion textured surface microstructure. Results indicate that the ultimate strength of the bulk materials is unchanged by ion texturing and that the microstructure will develop more rapidly if the substrate is heated prior to ion texturing.

Weigand, A. J.

Scanning Electron Microscopy Investigation of a Sample Depth Profile Through the Martian Meteorite Nakhla

The ongoing scientific debate as to whether or not the Martian meteorite ALH84001 contained evidence of possible biogenic activities showed the need to establish consistent methods to ascertain the origin of such evidence. To distinguish between terrestrial organic material/microbial contaminants and possible indigenous microbiota within meteorites is therefore crucial. With this in mind a depth profile consisting of four samples from a new sample allocation of Martian meteorite Nakhla was investigated using scanning electron microscopy (SEM) and energy dispersive X-ray analysis. SEM imaging of freshly broken fractured chips revealed structures strongly recent terrestrial microorganisms, in some cases showing evidence of active growth. This conclusion was supported by EDX analysis, which showed the presence of carbon associated with these structures, we concluded that these structures represent recent terrestrial contaminants rather than structures indigenous to the meteorite. Page

Toporski, Jan

Coaxial carbon plasma gun deposition of amorphous carbon films

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Sater, D. M.

Scanning electron microscopy of the vestibular end organs

The vestibular end organs, after chemical fixation, were freeze dried, coated with gold and palladium, and studied in the scanning microscope. Scanning microscopy gives a good three dimensional view of the sensory areas and allows study of both gross anatomy and microstructures. Cross anatomical features of the structure of the ampullae are demonstrated. The form of the statoconia in different species of animals is shown. New aspects of the structure of the sensory hairs are revealed. The hair bundles in the central areas of the cristae and in the striola of the maculae differ structurally from the hair bundles at the periphery of the sensory regions. Furthermore, some hair bundles consisting of very short stereocilia were observed. The relationship between the cupula and the statoconial membrane to the epithelial surface is discussed.

Lindeman, H. H.

Effects of radiation upon the light-sensing elements of the retina as characterized by scanning electron microscopy

A model system using Necturus maculosus, the common mudpuppy, was established for evaluating effects of radiation upon the light-sensing elements of the retina. Accelerated heavy ions of helium and neon from the Berkeley Bevalac were used. A number of criteria were chosen to characterize radiation damage by observing morphological changes with the scanning electron microscope. The studies indicated retina sensitivity to high-LET (neon) particles at radiation levels below 10 rads (7 particles per visual element) whereas no significant effects were seen from fast helium ions below 50 rads.

Malachowski, M. J.

Nondestructive determination of the depth of planar p-n junctions by scanning electron microscopy

A method was developed for measuring nondestructively the depth of planar p-n junctions in simple devices as well as in integrated-circuit structures with the electron-beam induced current (EBIC) by scanning parallel to the junction in a scanning electron microscope (SEM). The results were found to be in good agreement with those obtained by the commonly used destructive method of lapping at an angle to the junction and staining to reveal the junction.

Chi, J.-Y.

Moessbauer spectroscopy and scanning electron microscopy of the Murchison meteorite

Meteorites provide a wealth of information about the solar system's formation, since they have similar building blocks as the Earth's crust but have been virtually unaltered since their formation. Some stony meteorites contain minerals and silicate inclusions, called chondrules, in the matrix. Utilizing Moessbauer spectroscopy, we identified minerals in the Murchison meteorite, a carbonaceous chondritic meteorite, by the gamma ray resonance lines observed. Absorption patterns of the spectra were found due to the minerals olivine and phyllosilicate. We used a scanning electron microscope to describe the structure of the chondrules in the Murchison meteorite. The chondrules were found to be deformed due to weathering of the meteorite. Diameters varied in size from 0.2 to 0.5 mm. Further enhancement of the microscopic imagery using a digital image processor was used to describe the physical characteristics of the inclusions.

Brown, Christopher L.

Low voltage scanning electron microscopy of interplanetary dust particles

The resolution of available low-voltage SEM (LVSEM) models used in the characterization of interplanetary dust particles (IDPs) is limited by a number of factors including energy spread in the electron source, beam brightness, scanning electron detector geometry, and various lens aberrations. This paper describes an improved model of LVSEM which offers an increased resolution at low voltage. The improvements include a cold cathode FE source which has an extremely low inherent energy spread and high brightness, a second condenser lens to converge the beam and maintain an optimum aperture half-angle, and a detector optimized for low-voltage scanning-electron collection. To reduce lens aberrations, the specimen is immersed in the objective lens field. The features of several IDP samples observed using the images obtained with this LVSEM model are described.

Blake, D. F.

Visualization of Microbial Biomarkers by Scanning Electron Microscopy

We are developing tools to link the biochemical structure of selected biomarkers with putative biogenic structures observed in mineralized samples. The detection of evidence of life on Mars and other planets will rely on methods that can discriminate compounds formed exclusively by living organisms. While biogenic compounds, such as amino acids and nucleotides have been discovered in extraterrestrial sources, such as meteorites and comets, their formation can be explained by abiotic means. The formation of cellular structures, or more elaborate organic molecules, such as complex lipids, proteins or nucleic acids, however, is strongly correlated to the presence of even the most primitive life processes. Recent evidence lends support to the hypothesis that life may have once existed on Mars. Carbonate globules and ppm concentrations of polycyclic aromatic hydrocarbons (PAHs) have been described in ALH84001, a meteorite originating from Mars ejecta captured by Earth over 13,000 years ago. The localized high concentration of PAHs that follow an increasing gradient from the intact fusion crust towards the interior corresponds to microgram quantities of hydrocarbon. Even though ALH84001 and other similar meteorites have withstood the forces capable of ejecting rock through Mars' escape velocity, upon entering Earth's atmosphere, their core temperatures are likely not to have been raised significantly, as evidenced by the survival of remanent magnetic signatures. Ideal biomarkers of ancient or modern biological life would include molecules that are (or were) pervasive and highly resistant to degradation. Also, requisite methods of detection should be simple, extremely sensitive and broadly inclusive (NASA SP-530). Lipopolysaccharide (LPS), peptidoglycan or pseudopeptidoglycan and beta-glucan are microbial cell wall components which together cover the entire microbial spectrum of eubacteria, archea and fungi. They are all remarkably resistant to thermal degradation. Fortunately, many antimicrobial defense systems of higher organisms require sensitive detection to combat microbial pathogens. We employ here the primitive immune system of the evolutionarily ancient horseshoe crab, Limulus polyphemus. This species relies on multi-enzyme signal amplification detection of cell wall molecules and they can be applied to the development of useful detectors of life. An extension of this work includes the visualization of microbial signatures by labeling LAL components with chromogenic or electron dense markers. The protein Limulus Anti-LPS Factor (LALF) has an extremely high affinity for LPS. By coupling LALF binding with colloidal gold labels we demonstrate a correlation of the structures visible by electron microscopy with biochemical evidence of microbial cell wall materials. Pure silica particles were mixed with cultures of E. coli (10(exp 6) cfu/mL). Samples were washed sequentially with buffered saline, LALF, antibody to LALF and finally colloidal gold-labeled Protein A. Negative controls were not exposed to E. coli but received identical treatment otherwise. Samples were coated with carbon and imaged on a JEOL JSM-840 scanning electron microscope with LaB6 source in the back scatter mode with the JEOL annular back scatter detector. 20 nm-scale black spots in this contrast-reversed image originate from electrons back-scattered by gold atoms. Negative controls did not give any signal. Future work will expand application of this technique to soil simulants and mineralized rock samples.

Wainwright, Norman R.