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Heinemann, K.

Publications and source records attributed to Heinemann, K..

At least 37 records · Page 2
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NASA NTRS1980

Direct /TEM/ observation of the catalytic oxidation of amorphous carbon by Pd particles

The catalytic oxidation of amorphous carbon substrates by Pd particles is observed by in situ transmission electron microscopy. Various modes of selective attack of the carbon substrate in the immediate neighborhood of Pd particles are observed, which can be correlated with different degrees of particle mobility. Using amorphous substrates we have been able to demonstrate that the particle-substrate interaction is influenced by the structure of the particle. This has not previously been noted.

Moorhead, R. D.↗
NASA NTRS1979

Crystallography of decahedral and icosahedral particles. II - High symmetry orientations

Based on the exact crystal structure of decahedral and icosahedral particles, high energy electron diffraction patterns and image profiles have been derived for various high symmetry orientations of the particles with respect to the incident beam. These results form a basis for the identification of small metal particle structures with advanced methods of transmission electron microscopy.

Yang, C. Y.↗
NASA NTRS1979

The structure of small, vapor-deposited particles. II - Experimental study of particles with hexagonal profile

'Multiply-twinned' gold particles with hexagonal bright field TEM profile were determined to be icosahedra composed of 20 identical and twin-related tetrahedral building units that do not have an fcc structure. The crystal structure of these slightly deformed tetrahedra is rhombohedral. Experimental evidence supporting this particle model was obtained by selected-zone dark field and weak beam dark field electron microscopy. In conjunction with the results of part I, it has been concluded that multiply-twinned gold particles of pentagonal or hexagonal profile that are found during the early stages of the vapor deposition growth process on alkali halide surfaces do not have an fcc crystal structure, which is in obvious contrast to the structure of bulk gold.

Yacaman, M. J.↗
NASA NTRS1979

A structural analysis of small vapor-deposited 'multiply twinned' gold particles

High resolution selected zone dark field, Bragg reflection imaging and weak beam dark field techniques of transmission electron microscopy were used to determine the structure of small gold particles vapor deposited on NaCl substrates. Attention was focused on the analysis of those particles in the 50-150 A range that have pentagonal or hexagonal bright field profiles. These particles have been previously described as multiply twinned crystallites composed of face-centered cubic tetrahedra. The experimental evidence of the present studies can be interpreted on the assumption that the particle structure is a regular icosahedron or decahedron for the hexagonal or the pentagonal particles respectively. The icosahedron is a multiply twinned rhombohedral crystal and the decahedron is a multiply twinned body-centered orthorhombic crystal, each of which constitutes a slight distortion from the face-centered cubic structure.

Yang, C. Y.↗
NASA NTRS1977

In situ oxidation studies on /001/ copper-nickel alloy thin films

High-resolution transmission electron microscopy studies are reported of (001)-oriented single crystalline thin films of Cu-3%Ni, Cu-4.6%Ni, and Cu-50%Ni alloy which were prepared by vapor deposition onto (001) NaCl substrates and subsequently annealed at around 1100 K and oxidized at 725 K at low oxygen partial pressure. At all alloy concentrations, Cu2O and NiO nucleated and grew independently without the formation of mixed oxides. The shape and growth rates of Cu2O nuclei were similar to rates found earlier. For low-nickel alloy concentrations, the NiO nuclei were larger and the number density of NiO was less than that of Cu-50%Ni films for which the shape and growth rates of NiO were identical to those for pure nickel films. Phenomena involving a reduced induction period, surface precipitation, and through-thickness growth are also described. The results are consistent with previously established oxidation mechanisms for pure copper and pure nickel films.

Heinemann, K.↗
NASA NTRS1976

Electron microscope aperture system

An electron microscope including an electron source, a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen, and an objective lens having an annular objective aperture, for focusing electrons passing through the specimen onto an image plane are described. The invention also entails a method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques.

Heinemann, K.↗
NASA NTRS1976

Oxidation of metals and alloys in controlled atmospheres using in situ transmission electron microscopy and Auger spectrography

Single-crystalline thin films of copper were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of .005 Torr in situ in a high-resolution electron microscope. The specimens were prepared by epitaxial vapor deposition onto polished 100 and 110 faces of rocksalt and mounted in a hot stage inside an ultra-high-vacuum specimen chamber of the microscope. Large amounts of sulfur, carbon, and oxygen were detected by Auger electron spectroscopy on the surface of the as-received films and were removed in situ by ion-sputter etching immediately prior to the oxidation. The nucleation and growth characteristics of Cu2O on Cu were studied. Results show that neither stacking faults nor dislocations are associated with the Cu2O nucleation sites. The growth of Cu2O nuclei is linear with time. The experimental findings, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving (a) the formation of a surface-charge layer, (b) oxygen saturation in the metal and (c) nucleation, followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Rao, D. B.↗
NASA NTRS1976

In situ investigation of the mobility of small gold clusters on cleaved MgO surfaces

The mobility of small clusters of gold (about 10 A in diameter) on electron-beam-cleaved MgO surfaces was studied by in situ transmission electron microscopy under controlled vacuum and temperature conditions. During the first 10 min following a deposition at room temperature, over 10 per cent of the crystallites moved over short distances (about 20 A) discontinuously, with a velocity greater than 150 A/sec. Eighty per cent of the mobility events were characterized by the avoidance of proximity of other crystallites, and this was tentatively explained as the result of repulsive elastic forces between the interacting crystallites.

Metois, J. J.↗
NASA NTRS1976

Direct observation of small cluster mobility and ripening

Direct evidence is reported for the simultaneous occurrence of Ostwald ripening and short-distance cluster mobility during annealing of discontinuous metal films on clean amorphous substrates. The annealing characteristics of very thin particulate deposits of silver on amorphized clean surfaces of single-crystalline thin graphite substrates have been studied by in situ transmission electron microscopy (TEM) under controlled environmental conditions in the temperature range from 25 to 450 C. It was possible to monitor all stages of the experiments by TEM observation of the same specimen area. Slow Ostwald ripening was found to occur over the entire temperature range, but the overriding surface transport mechanism was short-distance cluster mobility. This was concluded from in situ observations of individual particles during annealing and from measurements of cluster size distributions, cluster number densities, area coverages, and mean cluster diameters.

Heinemann, K.↗
NASA NTRS1975

Oxide nucleation on thin films of copper during in situ oxidation in an electron microscope

Single-crystal copper thin films were oxidized at an isothermal temperature of 425 C and at an oxygen partial pressure of 0.005 torr. Specimens were prepared by epitaxial vapor deposition onto polished faces of rocksalt and were mounted in a hot stage inside the ultrahigh-vacuum chamber of a high-resolution electron microscope. An induction period of roughly 30 min was established which was independent of the film thickness but depended strongly on the oxygen partial pressure and to exposure to oxygen prior to oxidation. Neither stacking faults nor dislocations were found to be associated with the Cu2O nucleation sites. The experimental data, including results from oxygen dissolution experiments and from repetitive oxidation-reduction-oxidation sequences, fit well into the framework of an oxidation process involving the formation of a surface charge layer, oxygen saturation of the metal with formation of a supersaturated zone near the surface, and nucleation followed by surface diffusion of oxygen and bulk diffusion of copper for lateral and vertical oxide growth, respectively.

Heinemann, K.↗
NASA NTRS1975

Direct observation of small cluster mobility and ripening

Direct evidence is reported for the simultaneous occurrence of Ostwald ripening and short-distance cluster mobility during annealing of discontinuous metal films on clean amorphous substrates. The annealing characteristics of very thin particulate deposits of silver on amorphized clean surfaces of single crystalline thin graphite substrates were studied by in-situ transmission electron microscopy (TEM) under controlled environmental conditions (residual gas pressure of 10 to the minus 9th power torr) in the temperature range from 25 to 450 C. Sputter cleaning of the substrate surface, metal deposition, and annealing were monitored by TEM observation. Pseudostereographic presentation of micrographs in different annealing stages, the observation of the annealing behavior at cast shadow edges, and measurements with an electronic image analyzing system were employed to aid the visual perception and the analysis of changes in deposit structure recorded during annealing. Slow Ostwald ripening was found to occur in the entire temperature range, but the overriding surface transport mechanism was short-distance cluster mobility.

Heinemann, K.↗
NASA NTRS1974

Method of forming aperture plate for electron microscope

An electron microscope is described with an electron source a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen. It also has objective lens with an annular objective aperture, for focusing electrons passing through the specimen onto an image plane. A method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques is included.

Heinemann, K.↗
NASA NTRS1974

Summary of in situ epitaxial nucleation and growth measurements

In situ nucleation and growth measurements of Ag and Au on single-crystal PbSe thin films were made using a transmission electron microscope. Properties studied were polymorphism, crystalline perfection, and the stoichiometric composition of the initial and the autoepitaxially thickened PbSe substrates. The quantitative nucleation and cluster growth measurements were limited to low-saturation conditions. The epitaxial orientations are discussed, and evidence is presented as to the stage of deposition at which the epitaxial order for Ag is introduced. Strong substrate/overgrowth interaction manifested itself by alloying and interdiffusion.

Poppa, H.↗
NASA NTRS1973

In situ sputter cleaning of thin film metal substrates for UHV-TEM corrosion studies.

A prerequisite for conducting valid corrosion experiments by in situ electron microscopy techniques is not only the achievement of UHV background pressure conditions at the site of the specimen but also the ability to clean the surface of the thin metal substrate specimen before initiation of the corrosive interaction. A miniaturized simple ion gun has been constructed for this purpose. The gun is small enough to be incorporated into an UHV electron microscope specimen chamber with hot stage in such a way as to permit bombardment of the substrate specimen while observing it by transmission electron microscopy TEM. It is shown that the ion beam generated is confined well enough to cause a sputtering removal of substrate material at a rate of approximately 5-10 A/min and to prevent the sputter deposition of contaminating material from the specimen holder.

Heinemann, K.↗