Search NASA⌕ Search

SEARCH · Search NASA

Results for “x-ray microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 325 records · Page 18

Below band-gap laser ablation of diamond for transmission electron microscopy

A 248 nm excimer laser was used to thin naturally occurring type 1a diamond substrates at normal and glancing (22 deg) incidence. Perforation of a 250-micron-thick substrate was achieved in about 15 min at normal incidence. While the substrate thinned at glancing incidence was found to have large electron-transparent areas, that thinned at normal incidence required additional argon-ion milling to achieve electron transparency. X-ray photoelectron spectroscopy of the back surface of the diamond failed to detect any graphite or glassy carbon, confirming that damage due to laser ablation occurs only at the incident surface. Samples prepared using this technique imaged in the transmission electron microscope were observed to have retained the nitrogen platelets characteristic of such type 1a diamonds.

George, T.↗

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗

Surface analyses of composites exposed to the space environment on LDEF

We have conducted a series of surface analyses on carbon fiber/polyarylacetylene matrix composites that were exposed to the space environment on the LDEF satellite. None of the composites were catastrophically damaged by nearly six years of exposure to the space environment. Composites on the leading edge exhibited about 5 mils of surface erosion, but trailing edge panels exhibited no physical appearance changes due to exposure. Scanning electron microscopy (SEM) was used to show that the erosion morphology on the leading edge samples was dominated by crevasses parallel to the fibers with triangular cross sections 10 to 100 microns in depth. The edges of the crevasses were well defined and penetrated through both matrix and fiber. The data suggest that the carbon fibers are playing a significant role in crevasse initiation and/or enlargement, and in the overall erosion rate of the composite. X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS) results showed the presence of silicone and hydrocarbon contamination from in-flight sources. The role of contamination in crevasse initiation and enlargement is unknown at this time. These LDEF results demonstrate that the prediction of long term atomic oxygen erosion morphology for composite materials from erosion data obtained on short Space Shuttle missions is difficult. A better understanding of other factors such as thermal cycling and UV exposure which may influence erosion is necessary to improve the accuracy of the predictions.

Mallon, Joseph J.↗

Surface analyses of composites exposed to the space environment on LDEF

A series of surface analyses on carbon fiber/poly(arylacetylene) (PAA) matrix composites that were exposed to the space environment on the Long Duration Exposure Facility (LDEF) satellite were conducted. These composite panels were arranged in pairs on both the leading edge and trailing edge of LDEF. None of the composites were catastrophically damaged by nearly six years of exposure to the space environment. Composites on the leading edge exhibited from 25 to 125 microns of surface erosion, but trailing edge panels exhibited no physical appearance changes due to exposure. Scanning electron microscopy (SEM) was used to show that the erosion morphology on the leading edge samples was dominated by crevasses parallel to the fibers with triangular cross sections 10 to 100 microns in depth. The edges of the crevasses were well defined and penetrated through both matrix and fiber. The data suggest that the carbon fibers are playing an important role in crevasse initiation and/or enlargement, and in the overall erosion rate of the composite. X-ray photoelectron spectroscopy (XPS) and energy dispersive x-ray spectroscopy (EDS) results showed contamination from in-flight sources of silicone.

Mallon, Joseph J.↗

A Novel Microcharacterization Technique in the Measurement of Strain and Orientation Gradient in Advanced Materials

Representation of morphology and evolution of the microstructure during processing and their relation to properties requires proper experimental techniques. Residual strains, lattice distortion, and texture (micro-texture) at the interface and the matrix of a layered structure or a functionally gradient material and their variation are among parameters important in materials characterization but hard to measure with present experimental techniques. Current techniques available to measure changes in interred material parameters (residual stress, micro-texture, microplasticity) produce results which are either qualitative or unreliable. This problem becomes even more complicated in the case of a temperature variation. These parameters affect many of the mechanical properties of advanced materials including stress-strain relation, ductility, creep, and fatigue. A review of some novel experimental techniques using recent advances in electron microscopy is presented here to measure internal stress, (micro)texture, interracial strength and (sub)grain formation and realignment. Two of these techniques are combined in the chamber of an Environmental Scanning Electron Microscope to measure strain and orientation gradients in advanced materials. These techniques which include Backscattered Kikuchi Diffractometry (BKD) and Microscopic Strain Field Analysis are used to characterize metallic and intermetallic matrix composites and superplastic materials. These techniques are compared with the more conventional x-ray diffraction and indentation techniques.

Garmestai, H.↗

Laboratory Investigation of the Growth and Crystal Structure of Nitric Acid Hydrates by Transmission Electron Microscopy (TEM)

A great deal of recent laboratory work has focussed on the characterization of the nitric acid hydrates, thought to be present in type I Polar Stratospheric Clouds (PSCs). Phase relationships and vapor pressure measurements (1-3) and infrared characterizations (4-5) have been made. However, the observed properties of crystalline solids (composition, melting point, vapor pressure, surface reactivity, thermodynamic stability, extent of solid solution with other components, etc.) are controlled by their crystal structure. The only means of unequivocal structural identification for crystalline solids is diffraction (using electrons, X-rays, neutrons, etc.). Other observed properties of crystalline solids, such as their infrared spectra, their vapor pressure as a function of temperature, etc. yield only indirect information about what phases are present, their relative proportions, or whether they are crystalline or amorphous.

Blake, David F.↗

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗

Electron spectroscopy analysis

The Surface Science Laboratories at the University of Alabama in Huntsville (UAH) are equipped with x-ray photoelectron spectroscopy (XPS or ESCA) and Auger electron spectroscopy (AES) facilities. These techniques provide information from the uppermost atomic layers of a sample, and are thus truly surface sensitive. XPS provides both elemental and chemical state information without restriction on the type of material that can be analyzed. The sample is placed into an ultra high vacuum (UHV) chamber and irradiated with x-rays which cause the ejection of photoelectrons from the sample surface. Since x-rays do not normally cause charging problems or beam damage, XPS is applicable to a wide range of samples including metals, polymers, catalysts, and fibers. AES uses a beam of high energy electrons as a surface probe. Following electronic rearrangements within excited atoms by this probe, Auger electrons characteristic of each element present are emitted from the sample. The main advantage of electron induced AES is that the electron beam can be focused down to a small diameter and localized analysis can be carried out. On the rastering of this beam synchronously with a video display using established scanning electron microscopy techniques, physical images and chemical distribution maps of the surface can be produced. Thus very small features, such as electronic circuit elements or corrosion pits in metals, can be investigated. Facilities are available on both XPS and AES instruments for depth-profiling of materials, using a beam of argon ions to sputter away consecutive layers of material to reveal sub-surface (and even semi-bulk) analyses.

Gregory, John C.↗

A study of thermal transitions in a new semicrystalline thermoplastic polyimide

A polyimide derive from 4,4'-isophthaloyl diphthalic anhydride (IDPA) and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene (1,3-BABB) having semicrystalline behavior was prepared and characterized by differential scanning calorimetry (DSC) and wide angle X-ray scattering (WAXS). Thus a poly(amic acid) film cured in air for one hour each at 100 and 200 C displayed an endotherm at 286 C, followed by a crystallization exotherm at 317 C, and a second melting transition at 350 C. The 286 C melting point appeared to result from earlier solvent-induced crystallization. Films cast from DMAc, air dried, and soaked in methylene chloride could not be induced into semicrystallinity. The fully cured polyimide has a Tg of 216 C. Films heated to temperatures as high as 100 C for one hour in air were transparent and light yellow in color. Those films heated to or above 125 C were translucent. Polarized light microscopy revealed the presence of spherulites 608 micrometers in diameter in a sample cured to 275 C in air. Two film samples, one cured to 275 and the other to 325 C, were evaluated for tensile and ultimate strength, modulus, and percent elongation at 25 and 200 C. These values remained essentially constant at each test temperature.

Pratt, J. Richard↗

Crystallization Kinetics of Barium and Strontium Aluminosilicate Glasses of Feldspar Composition

Crystallization kinetics of BaO.Al2O3.2SiO2 (BAS) and SrO.Al2O3.2SiO2 (SAS) glasses in bulk and powder forms have been studied by non-isothermal differential scanning calorimetry (DSC). The crystal growth activation energies were evaluated to be 473 and 451 kJ/mol for bulk samples and 560 and 534 kJ/mol for powder specimens in BAS and SAS glasses, respectively. Development of crystalline phases on thermal treatments of glasses at various temperatures has been followed by powder x-ray diffraction. Powder samples crystallized at lower temperatures than the bulk and the crystallization temperature was lower for SAS glass than BAS. Crystallization in both glasses appeared to be surface nucleated. The high temperature phase hexacelsian, MAl2Si2O8 (M = Ba or Sr), crystallized first by nucleating preferentially on the glass surface. Also, monoclinic celsian does not nucleate directly in the glass, but is formed at higher temperatures from the transformation of the metastable hexagonal phase. In SAS the transformation to monoclinic celsian occurred rapidly after 1 h at 1100 C. In contrast, in BAS this transformation is sluggish and difficult and did not go to completion even after 10 h heat treatment at 1400 C. The crystal growth morphologies in the glasses have been observed by optical microscopy. Some of the physical properties of the two glasses are also reported.

Hyatt, Mark J.↗

Investigation of nucleation and growth processes of diamond films by atomic force microscopy

The nucleation and growth of plasma enhanced chemical vapor deposited (PECVD) polycrystalline diamond films were studied using atomic force microscopy (AFM). AFM images were obtained for: (1) nucleated diamond films produced from depositions that were terminated during the initial stages of growth, (2) the silicon substrate-diamond film interface side of diamond films (1-4 micrometers thick) removed from the original surface of the substrate, and (3) cross-sectional fracture surface of the film, including the Si/diamond interface. Pronounced tip effects were observed for early-stage diamond nucleation attributed to tip convolution in the AFM images. AFM images of the films cross-section and interface however were not affected by tip convolution, and the images indicate that the surface of the silicon substrate is initially covered by small grained polycrystalline-like film and the formation of this precursor film is followed by nucleation of the diamond film on top of this layer. X-ray photoelectron spectroscoy (XPS) spectra indicates that some silicon carbide is present in the precursor layer.

George, M. A.↗

Investigation of nucleation and growth processes of diamond films by atomic force microscopy

The nucleation and growth of plasma-enhanced chemical-vapor deposited polycrystalline diamond films were studied using atomic force microscopy (AFM). AFM images were obtained for (1) nucleated diamond films produced from depositions that were terminated during the initial stages of growth, (2) the silicon substrate-diamond film interface side of diamond films (1-4 micrometers thick) removed from the original surface of the substrate, and (3) the cross-sectional fracture surface of the film, including the Si/diamond interface. Pronounced tip effects were observed for early-stage diamond nucleation attributed to tip convolution in the AFM images. AFM images of the film's cross section and interface, however, were not highly affected by tip convolution, and the images indicate that the surface of the silicon substrate is initially covered by a small grained polycrystalline-like film and the formation of this precursor film is followed by nucleation of the diamond film on top of this layer. X-ray photoelectron spectroscopy spectra indicate that some silicon carbide is present in the precursor layer.

George, M. A.↗

Soft x ray window encapsulant for HgI2 detectors

HgI2 is an excellent semiconductor material for a low energy, room temperature x-ray spectrometer. The high values of the atomic numbers for its constituent elements gives high x-ray and gamma ray stopping power. The band gap of HgI2 is significantly higher than other commonly used semiconductors. Owing to the large value band gap, the leakage current for HgI2 devices is smaller, thus allowing low noise performance. Devices fabricated from HgI2 crystals have demonstrated energy resolution sufficient to distinguish the x-ray emission from the neighboring elements on the periodic table. Also the power requirements of HgI2 are very low. These characteristics make a HgI2 spectrometer an ideal component in a satellite based detection system. Unfortunately, HgI2 crystals tend to deteriorate with time, even if protected by standard semiconductor encapsulants. This degradation ruins the performance of the device in terms of its energy resolution and pulse amplitude. The degrading mechanism is believed to be material loss occurring from below the electrodes, due to high vapor pressure of HgI2 at room temperature. To address this major obstacle to rapid expansion of HgI2 technology, a research program aimed at improving device stability by encapsulation with inert polymeric materials was carried out. The program focused specifically on optimizing the encapsulant materials and their deposition techniques. The principal objectives for this program were device encapsulation, device testing, and accelerated testing to ensure very long term stability of these high resolution sensors. A variety of encapsulants were investigated with the selection criteria based on their chemical diffusion barrier properties, mechanical stability, reactivity, and morphology of encapsulant films. The investigation covered different classes of encapsulants including solvent based encapsulants, vapor deposited encapsulants, and plasma polymerized encapsulants. A variety of characterization techniques were employed to examine their effectiveness in stabilizing HgI2 devices; these included permeability evaluation, vacuum and heat testing, scanning electron microscopy (SEM) as well as studying the detector performance of coated detectors. The plasma polymerized films appear to have entirely solved the HgI2 degradation problem. Another achievement of this program was the development of an accelerated testing technique which correlates extremely well with long term tesing.

Entine, G.↗

The locations and amounts of endogenous ions and elements in the cap and elongating zone of horizontally oriented roots of Zea mays L.: an electron-probe EDS study

We used quantitative electron-probe energy-dispersive x-ray microanalysis to localize endogenous Na, Cl, K, P, S, Mg and Ca in cryofixed and freeze-dried cryosections of the cap (i.e. the putative site of graviperception) and elongating zone (i.e. site of gravicurvature) of horizontally oriented roots of Zea mays. Ca, Na, Cl, K and Mg accumulate along the lower side of caps of horizontally oriented roots. The most dramatic asymmetries of these ions occur in the apoplast, especially the mucilage. We could not detect any significant differences in the concentrations of these ions in the central cytoplasm of columella cells along the upper and lower sides of caps of horizontally-oriented roots. However, the increased amounts of Na, Cl, K and Mg in the longitudinal walls of columella cells along the lower side of the cap suggest that these ions may move down through the columella tissue of horizontally-oriented roots. Ca also accumulates (largely in the mucilage) along the lower side of the elongating zone of horizontally-oriented roots, while Na, P, Cl and K tend to accumulate along the upper side of the elongating zone. Of these ions, only K increases in concentration in the cytoplasm and longitudinal walls of cortical cells in the upper vs lower sides of the elongating zone. These results indicate that (1) gravity-induced asymmetries of ions differ significantly in the cap and elongating zone of graviresponding roots, (2) Ca accumulates along the lower side of the cap and elongating zone of graviresponding roots, (3) increased growth of the upper side of the elongating zone of horizontally-oriented roots correlates positively with increased amounts of K in the cytoplasm and longitudinal walls of cortical cells, and (4) the apoplast (especially the mucilage) may be an important component of the pathway via which ions move in graviresponding rots of Zea mays. These results are discussed relative to mechanisms for graviperception and gravicurvature of roots.

NASA Program Space Biology↗

Microscopic observations of X-ray and gamma-ray induced decomposition of ammonium perchlorate crystals

The X-ray and gamma-ray induced decomposition of ammonium perchlorate was studied by optical, transmission, and scanning electron microscopy. This material is a commonly used oxidizer in solid propellents which could be employed in deep-space probes, and where they will be subjected to a variety of radiations for as long as ten years. In some respects the radiation-induced damage closely resembles the effects produced by thermal decomposition, but in other respects the results differ markedly. Similar radiation and thermal effects include the following: (1) irregular or ill-defined circular etch pits are formed in both cases; (2) approximately the same size pits are produced; (3) the pit density is similar; (4) the c face is considerably more reactive than the m face; and (5) most importantly, many of the etch pits are aligned in crystallographic directions which are the same for thermal or radiolytic decomposition. Thus, dislocations play an important role in the radiolytic decomposition process.

Herley, P. J.↗

Highly oriented Tl2Ba2Ca2Cu3O10 thin films by pulsed laser evaporation

Superconducting thin films on MgO (100) substrates with nearly pure Tl2Ba2Ca2Cu3O10 (2:2:2:3) phase using pulsed laser evaporation and postannealing have been fabricated. The films had c axes perpendicular to the substrates. Superconducting films with onset temperatures of 125 K and zero resistance at 110 K were obtained. X-ray microprobe fluorescence measurements indicate that a typical composition of films is Tl(0.66)Ba(1.77)Ca(1.46)Cu3O(x) which is low in Tl compared to that expected for the 2:2:2:3 phase. A typical grain size is greater than 10 microns revealed by scanning electron microscopy.

Liou, S. H.↗

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.↗