Surface Composition of TiO2-Zn Nanotubes by NanoSIMS

MRS Advances ◽  
2016 ◽  
Vol 1 (46) ◽  
pp. 3151-3156
Author(s):  
Indu B Mishra ◽  
Diana Khusnutdinova ◽  
William T Petuskey
Keyword(s):  
Secondary Electron ◽  
High Spatial Resolution ◽  
Surface Composition ◽  
High Vacuum ◽  
Isotopic Analysis ◽  
Ultra High Vacuum ◽  
Actual Content ◽  
Before And After ◽  
Sims Analysis

ABSTRACTTitania nanotubes were prepared by anodic oxidation of Ti. The titania surfaces were partially coated with Zn by reacting zinc acetate with the nanotubes and then annealed. [1] An annealed nanotube cluster was placed carefully on a silicon wafer using tweezers. Secondary electron images were acquired by bombarding with Cs+ and observing the ejected OZn- and OTi- respectively. The SIMS analysis was done in ultra-high vacuum (∼ 10-10 Torr). The location of before and after the SIMS analysis was confirmed by scanning electron microscopy (SEM). Specific areas with various orientations (vertical and horizontal orientations) of the nanotubes were selected for the NanoSIMS 50L analysis. The NanoSIMS 50L is made by Ametek Cameca, Gennevillieres, France and is capable of doing in situ isotopic analysis of surfaces at high spatial resolution (25 nm2). The average ZnO/TiO was ∼1.8%, confirming the actual content of Zn used during synthesis of the nanotubes. Qualitatively, the TiO/ZnO ratio increased with increasing depth implying that ZnO concentration was decreasing as we probed into the nanotubes.

The Origins of High Spatial Resolution Secondary Electron Microscopy

1992 ◽  
Vol 295 ◽  
Author(s):  
M. R. Scheinfein ◽  
J. S. Drucker ◽  
J. Liu ◽  
J. K. Weiss ◽  
G. G. Hembree ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Spatial Resolution ◽  
Secondary Electron ◽  
High Spatial Resolution ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Generation Process ◽  
Secondary Electrons ◽  
Electron Generation ◽  
Secondary Electron Generation

AbstractThe secondary electron generation process is studied in an ultra-high vacuum scanning transmission electron microscope using electron coincidence spectroscopy. Production pathways for secondary electrons are determined by analyzing coincidences between secondary electrons and individual excitation events. The ultimate spatial resolution available in scanning electron microscopy is limited by the delocalization of the secondary electron generation process. This delocalization is studied using momentum resolved coincidence electron spectroscopy. The fraction of secondary electrons resulting from localized excitations can explain the high spatial resolution observed in secondary electron microscopy images.

μm-Scale Lateral Growth of Ga-Monolayers Observed In-Situ by Electron Microscopy

1989 ◽  
Vol 159 ◽  
Author(s):  
J. Osaka ◽  
N. Inoue
Keyword(s):  
Electron Microscopy ◽  
Secondary Electron ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Intensity Difference ◽  
Lateral Growth ◽  
Mbe Growth ◽  
Electron Intensity ◽  
Scanning Electron

ABSTRACTAn ultra high vacuum scanning electron microscope equipped to an MBE system is utilized to study a transient of a surface atomic structure during MBE growth of GaAs and AlGaAs by the alternate supply method. Lateral growth of a Ga-monolayer over microns is realized utilizing Ga droplets. This is confirmed by discriminating the Ga and As top layer by using the secondary electron intensity difference between the Ga and As top layer. The growth mechanism of the Ga monolayer is discussed based on the results.

Deuterium Out-Diffusion Kinetics in Magnesium-Doped GaN

2007 ◽  
Vol 994 ◽  
Author(s):  
Jacques Chevallier ◽  
François Jomard ◽  
Norbert H. Nickel ◽  
Philippe de Mierry ◽  
Sébastien Chenot ◽  
...  
Keyword(s):  
High Vacuum ◽  
Ultra High Vacuum ◽  
Diffusion Kinetics ◽  
First Order ◽  
Annealing Step ◽  
Before And After ◽  
Sims Analysis ◽  
Kinetics Of ◽  
Annealing Experiments ◽  
Mg Doped

AbstractA series of isothermal annealing experiments have been performed in the range 790–920°C under N2 flow in order to study the deuterium out-diffusion kinetics of Mg-doped GaN grown on sapphire under deuterated ammonia. The deuterium concentration was measured by SIMS analysis before and after each annealing step. The kinetics closely follow a first-order law. The activation energy related to the deuterium out-diffusion process is 3.1 eV. In addition, deuterium effusion measurements were performed measuring the molecular HD flux while the specimens were annealed in ultra high vacuum with a linear heating rate. In contrast to SIMS, this method detects the species that migrated out of the sample. Effusion peaks of the HD flux at 360 and 490°C are attributed to the fragmentation of adsorbed CHxDy complexes. The molecular HD flux starts increasing at 800°C which is the onset of the GaN decomposition and has its maximum at 920°C. This HD flux is accompanied by the desorption of H and D containing radicals and molecules desorbing above 900°C.

Structure of Palladium Single-Crystal Films Prepared by Flash Evaporation onto (001) NaCl Substrates

1970 ◽  
Vol 28 ◽  
pp. 456-457
Author(s):  
L. E. Murr ◽  
G. Wong
Keyword(s):  
Single Crystal ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
High Rate ◽  
Flash Evaporation ◽  
Optimum Load ◽  
Single Crystal Films ◽  
Crystal Films ◽  
A Current

Palladium single-crystal films have been prepared by Matthews in ultra-high vacuum by evaporation onto (001) NaCl substrates cleaved in-situ, and maintained at ∼ 350° C. Murr has also produced large-grained and single-crystal Pd films by high-rate evaporation onto (001) NaCl air-cleaved substrates at 350°C. In the present work, very large (∼ 3cm2), continuous single-crystal films of Pd have been prepared by flash evaporation onto air-cleaved (001) NaCl substrates at temperatures at or below 250°C. Evaporation rates estimated to be ≧ 2000 Å/sec, were obtained by effectively short-circuiting 1 mil tungsten evaporation boats in a self-regulating system which maintained an optimum load current of approximately 90 amperes; corresponding to a current density through the boat of ∼ 4 × 104 amperes/cm2.

Hetero-Epitaxy of Group Va Metals on Sapphire

1972 ◽  
Vol 30 ◽  
pp. 492-493
Author(s):  
J. E. O'Neal ◽  
J. J. Bellina ◽  
B. B. Rath
Keyword(s):  
Thermal Contact ◽  
High Vacuum ◽  
Electron Beam Evaporation ◽  
Ultra High Vacuum ◽  
Backing Plate ◽  
Sapphire Substrates ◽  
Deposition Parameters ◽  
Polishing Damage ◽  
Reflection Electron Diffraction

Thin films of the bcc metals vanadium, niobium and tantalum were epitaxially grown on (0001) and sapphire substrates. Prior to deposition, the mechanical polishing damage on the substrates was removed by an in-situ etch. The metal films were deposited by electron-beam evaporation in ultra-high vacuum. The substrates were heated by thermal contact with an electron-bombarded backing plate. The deposition parameters are summarized in Table 1.The films were replicated and examined by electron microscopy and their crystallographic orientation and texture were determined by reflection electron diffraction. Verneuil-grown and Czochralskigrown sapphire substrates of both orientations were employed for each evaporation. The orientation of the metal deposit was not affected by either increasing the density of sub-grain boundaries by about a factor of ten or decreasing the deposition rate by a factor of two. The results on growth epitaxy are summarized in Tables 2 and 3.

An in situ and ex situ TEM study of the formation of thin cobalt silicide films by molecular beam epitaxy on the silicon (100) surface

1988 ◽  
Vol 46 ◽  
pp. 884-885
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove ◽  
R. T. Tung
Keyword(s):  
Molecular Beam Epitaxy ◽  
Molecular Beam ◽  
Defect Density ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Metal Base ◽  
In Situ Experiments ◽  
Potential Applications

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.

Design of a UHV STEM for Through-The-Lens Electron Spectroscopy

1990 ◽  
Vol 48 (2) ◽  
pp. 380-381
Author(s):  
A. J. Bleeker ◽  
P. Kruit
Keyword(s):  
Secondary Electron ◽  
High Vacuum ◽  
Secondary Electron Emission ◽  
Auger Spectroscopy ◽  
Scanning Transmission Electron Microscope ◽  
Point Of View ◽  
Ultra High Vacuum ◽  
Scanning Transmission ◽  
Auger Spectra ◽  
Coincidence Measurements

Combining of the high spatial resolution of a Scanning Transmission Electron Microscope and the wealth of information from the secondary electrons and Auger spectra opens up new possibilities for materials research. In a prototype instrument at the Delft University of Technology we have shown that it is possible from the optical point of view to combine STEM and Auger spectroscopy [1]. With an Electron Energy Loss Spectrometer attached to the microscope it also became possible to perform coincidence measurements between the secondary electron signal and the EELS signal. We measured Auger spectra of carbon aluminium and Argon gas showing energy resolutions better than 1eV [2]. The coincidence measurements on carbon with a time resolution of 5 ns yielded basic insight in secondary electron emission processes [3]. However, for serious Auger spectroscopy, the specimen needs to be in Ultra High Vacuum. ( 10−10 Torr ). At this moment a new setup is in its last phase of construction.

Nucleation and initial growth of Pd2Si crystals on Si(111)

1993 ◽  
Vol 51 ◽  
pp. 844-845
Author(s):  
Xianghong Tong ◽  
Oliver Pohland ◽  
J. Murray Gibson
Keyword(s):  
High Vacuum ◽  
Dark Field ◽  
Ultra High Vacuum ◽  
Initial Growth ◽  
Surface And Interface ◽  
Dark Field Imaging ◽  
Transmission Electron ◽  
Initial Stage ◽  
Effect Of Surface

The nucleation and initial stage of Pd2Si crystals on Si(111) surface is studied in situ using an Ultra-High Vacuum (UHV) Transmission Electron Microscope (TEM). A modified JEOL 200CX TEM is used for the study. The Si(111) sample is prepared by chemical thinning and is cleaned inside the UHV chamber with base pressure of 1x10−9 τ. A Pd film of 20 Å thick is deposited on to the Si(111) sample in situ using a built-in mini evaporator. This room temperature deposited Pd film is thermally annealed subsequently to form Pd2Si crystals. Surface sensitive dark field imaging is used for the study to reveal the effect of surface and interface steps.The initial growth of the Pd2Si has three stages: nucleation, growth of the nuclei and coalescence of the nuclei. Our experiments shows that the nucleation of the Pd2Si crystal occurs randomly and almost instantaneously on the terraces upon thermal annealing or electron irradiation.

Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

1989 ◽  
Vol 47 ◽  
pp. 462-463
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Transmission Electron

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.

Modifications of a JEOL 2000EX TEM for insSitu surface studies

1993 ◽  
Vol 51 ◽  
pp. 640-641
Author(s):  
Michael T. Marshall ◽  
Xianghong Tong ◽  
J. Murray Gibson
Keyword(s):  
Electron Diffraction ◽  
Surface Science ◽  
Film Growth ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Transmission Electron ◽  
Fundamental Insight

We have modified a JEOL 2000EX Transmission Electron Microscope (TEM) to allow in-situ ultra-high vacuum (UHV) surface science experiments as well as transmission electron diffraction and imaging. Our goal is to support research in the areas of in-situ film growth, oxidation, and etching on semiconducter surfaces and, hence, gain fundamental insight of the structural components involved with these processes. The large volume chamber needed for such experiments limits the resolution to about 30 Å, primarily due to electron optics. Figure 1 shows the standard JEOL 2000EX TEM. The UHV chamber in figure 2 replaces the specimen area of the TEM, as shown in figure 3. The chamber is outfitted with Low Energy Electron Diffraction (LEED), Auger Electron Spectroscopy (AES), Residual Gas Analyzer (RGA), gas dosing, and evaporation sources. Reflection Electron Microscopy (REM) is also possible. This instrument is referred to as SHEBA (Surface High-energy Electron Beam Apparatus).The UHV chamber measures 800 mm in diameter and 400 mm in height. JEOL provided adapter flanges for the column.

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