Electron Holographic Characterization of Nano-Hetero Interface Effect in Gold Catalysts

2004 ◽  
Vol 839 ◽  
Author(s):  
S. Ichikawa ◽  
T. Akita ◽  
K. Okazaki ◽  
K. Tanaka ◽  
M. Kohyama

ABSTRACTWe investigated the atomic structure near the interface and the size dependence of the mean inner potential of gold in Au/TiO2 catalysts prepared by the deposition precipitation (DP) method and the vacuum evaporation (VE) method using high resolution electron microscopy (HREM) and electron holography. The TiO2 supports prepared by DP method and VE method are considered to have oxygen-rich surfaces and titanium-rich surfaces respectively. In case of the Au/TiO2 catalyst prepared by DP method, the mean inner potential of gold increased depending on the size of the particle. When the size of the gold particle is over 5nm, the mean inner potential of gold was the same as that of bulk Au. When the size is below 5nm, the mean inner potential became to increase. It increases suddenly over 40V, particularly in case of below 2nm. It indicates that the electronic state of gold on TiO2 changes from that of bulk state as the size decreases. On the other hand, the mean inner potential of gold in Au/TiO2 catalysts prepared by VE method also increased as the size decreased, but the behavior of the size dependence is different from that of DP method. The critical size of the mean inner potential change is around 3nm. The size of the gold particle was below 3nm, the mean inner potential of gold increased gradually. The mean inner potential of VE method is less than that of DP method with the same particle size in spite of the size below 3nm. The stoichiometry at the interface between Au and TiO2 should be one of the dominant reasons for the behavior difference of the size dependence of the mean inner potential between the preparations.

Author(s):  
Y. Cheng ◽  
J. Liu ◽  
M.B. Stearns ◽  
D.G. Steams

The Rh/Si multilayer (ML) thin films are promising optical elements for soft x-rays since they have a calculated normal incidence reflectivity of ∼60% at a x-ray wavelength of ∼13 nm. However, a reflectivity of only 28% has been attained to date for ML fabricated by dc magnetron sputtering. In order to determine the cause of this degraded reflectivity the microstructure of this ML was examined on cross-sectional specimens with two high-resolution electron microscopy (HREM and HAADF) techniques.Cross-sectional specimens were made from an as-prepared ML sample and from the same ML annealed at 298 °C for 1 and 100 hours. The specimens were imaged using a JEM-4000EX TEM operating at 400 kV with a point-to-point resolution of better than 0.17 nm. The specimens were viewed along Si [110] projection of the substrate, with the (001) Si surface plane parallel to the beam direction.


Author(s):  
K. J. Morrissey

Grain boundaries and interfaces play an important role in determining both physical and mechanical properties of polycrystalline materials. To understand how the structure of interfaces can be controlled to optimize properties, it is necessary to understand and be able to predict their crystal chemistry. Transmission electron microscopy (TEM), analytical electron microscopy (AEM,), and high resolution electron microscopy (HREM) are essential tools for the characterization of the different types of interfaces which exist in ceramic systems. The purpose of this paper is to illustrate some specific areas in which understanding interface structure is important. Interfaces in sintered bodies, materials produced through phase transformation and electronic packaging are discussed.


Author(s):  
M. José-Yacamán

Electron microscopy is a fundamental tool in materials characterization. In the case of nanostructured materials we are looking for features with a size in the nanometer range. Therefore often the conventional TEM techniques are not enough for characterization of nanophases. High Resolution Electron Microscopy (HREM), is a key technique in order to characterize those materials with a resolution of ~ 1.7A. High resolution studies of metallic nanostructured materials has been also reported in the literature. It is concluded that boundaries in nanophase materials are similar in structure to the regular grain boundaries. That work therefore did not confirm the early hipothesis on the field that grain boundaries in nanostructured materials have a special behavior. We will show in this paper that by a combination of HREM image processing, and image calculations, it is possible to prove that small particles and coalesced grains have a significant surface roughness, as well as large internal strain.


Author(s):  
Margaret L. Sattler ◽  
Michael A. O'Keefe

Multilayered materials have been fabricated with such high perfection that individual layers having two atoms deep are possible. Characterization of the interfaces between these multilayers is achieved by high resolution electron microscopy and Figure 1a shows the cross-section of one type of multilayer. The production of such an image with atomically smooth interfaces depends upon certain factors which are not always reliable. For example, diffusion at the interface may produce complex interlayers which are important to the properties of the multilayers but which are difficult to observe. Similarly, anomalous conditions of imaging or of fabrication may occur which produce images having similar traits as the diffusion case above, e.g., imaging on a tilted/bent multilayer sample (Figure 1b) or deposition upon an unaligned substrate (Figure 1c). It is the purpose of this study to simulate the image of the perfect multilayer interface and to compare with simulated images having these anomalies.


Author(s):  
L. D. Marks ◽  
J. P. Zhang

A not uncommon question in electron microscopy is what happens to the momentum transferred by the electron beam to a crystal. If the beam passes through a crystal and is preferentially diffracted in one direction, is the momentum ’lost’ by the beam transferred to the crystal? Newton’s third law implies that this must be the case. Some experimental observations also indicate that this is the case; for instance, with small particles if the particles are supported on the top surface of a film they often do not line up on the zone axis, but if they are on the bottom they do. However, if momentum is transferred to the crystal, then surely we are dealing with inelastic scattering, not elastic scattering and is not the scattering probability different? In addition, normally we consider inelastic scatter as incoherent, and therefore the part of the electron wave that is inelastically scattered will not coherently interfere with the part of the wave that is scattered; but, electron holography and high resolution electron microscopy work so the wave passing through a specimen must be coherent with the wave that does not pass through the specimen.


2002 ◽  
Vol 727 ◽  
Author(s):  
S. Ichikawa ◽  
T. Akita ◽  
M. Okumura ◽  
M. Haruta ◽  
K. Tanaka

AbstractThe catalytic properties of nanostructured gold catalyst are known to depend on the size of the gold particles and to be activated when the size decreases to a few nanometers. We investigated the size dependence of the three-dimensional nanostructure on the mean inner potential of gold catalysts supported on titanium oxide using electron holography and high-resolution electron microscopy (HREM). The contact angle of the gold particles on the titanium oxide tended to be over 90° for gold particles with a size of over 5 nm, and below 90° for a size of below 2 nm. This decreasing change in the contact angle (morphology) acts to increase the perimeter and hence the area of the interface between the gold and titanium oxide support, which is considered to be an active site for CO oxidation. The mean inner potential of the gold particles also changed as their size decreased. The value of the inner potential of gold, which is approximately 25 V in bulk state, rose to over 40 V when the size of the gold particles was less than 2 nm. This phenomenon indicates the existence of a charge transfer at the interface between gold and titanium oxide. The 3-D structure change and the inner potential change should be attributed to the specific electronic structure at the interface, owing to both the “nano size effect” and the “hetero-interface effect.”


2001 ◽  
Vol 703 ◽  
Author(s):  
André Heinemann ◽  
Helmut Hermann ◽  
Albrecht Wiedenmann ◽  
Norbert Mattern ◽  
Uta Kühn ◽  
...  

ABSTRACTBulk amorphous Zr54.5 Ti7.5Al10Cu20Ni8 is investigated by means of smal-angle neutron scattering (SANS), differential-scanning calorimetry (DSC), high-resolution electron microscopy (HREM) and other methods. The formation of ultrafine nanostructures in the glassy phase is observed and explained by a new model. Structura fluctuations of randomly distributed partialy ordered domains grow during annealing just below the glass transition temperature by local re-ordering. During anneaing the DSC gives evidence for a increasing volume fraction of the localy ordered domains. At high volume fractions of impinging domains a percolation threshold on the interconnected domain boundaries occurs and enhanced diffusion becomes possible. At that stage SANS measurements lead to satistically significant scattering data. The SANS signals are anayzed in terms of a model taking into account spherica particles surrounded by diffusion zones and interparticle interference effects. The mean radius of the nanocrystaline particles is determined to 1 nm and the mean thickness of the depletion zone is 2 nm. The upper limit for the volume fraction after annealing at 653 K for 4hours is about 20 %. Electron microscopy confirms the size and shows that the particle are crystaline.


2019 ◽  
Vol 9 (11) ◽  
pp. 312 ◽  
Author(s):  
Vega-Zelaya ◽  
Torres ◽  
Navas ◽  
Pastor

Deep brain stimulation (DBS) requires precise localization, which is especially difficult at the thalamus, and even more difficult in anesthetized patients. We aimed to characterize the neurophysiological properties of the ventral intermediate (V.im), ventral caudal (V.c), and centromedian parvo (Ce.pc) and the magnocellular (Ce.mc) thalamic nuclei. We obtained microelectrode recordings from five patients with refractory epilepsy under general anesthesia. Somatosensory evoked potentials recorded by microelectrodes were used to identify the V.c nucleus. Trajectories were reconstructed off-line to identify the nucleus recorded, and the amplitude of the action potential (AP) and the tonic (i.e., mean frequency, density, probability of interspike interval) and phasic (i.e., burst index, pause index, and pause ratio) properties of the pattern discharges were analyzed. The Mahalanobis metric was used to evaluate the similarity of the patterns. The mean AP amplitude was higher for the V.im nucleus (172.7 ± 7.6 µV) than for the other nuclei, and the mean frequency was lower for the Ce.pc nucleus (7.2 ± 0.8 Hz) and higher for the V.c nucleus (11.9 ± 0.8 Hz) than for the other nuclei. The phasic properties showed a bursting pattern for the V.c nucleus and a tonic pattern for the centromedian and V.im nuclei. The Mahalanobis distance was the shortest for the V.im/V.c and Ce.mp/Ce.pc pairs. Therefore, the different properties of the thalamic nuclei, even for patients under general anesthesia, can be used to positively define the recorded structure, improving the exactness of electrode placement in DBS.


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