Surface Reconstruction and Oxide Nucleation Due to Oxygen Interaction with Cu(001) Observed by In Situ Ultra-High Vacuum Transmission Electron Microscopy

1998 ◽  
Vol 4 (3) ◽  
pp. 334-339 ◽  
Author(s):  
Judith C. Yang ◽  
Mark Yeadon ◽  
Borys Kolasa ◽  
J. Murray Gibson
Keyword(s):  
Surface Reconstruction ◽  
Dwell Time ◽  
High Vacuum ◽  
Copper Surface ◽  
Ultra High Vacuum ◽  
Oxide Formation ◽  
Transmission Electron ◽  
Oxygen Gas ◽  
Oxygen Interaction

Reconstruction of the Cu(001) surface due to oxygen gas impingement on a clean copper surface was directly observed by in situ UHV-TEM. Strain contrast between differently oriented surface reconstruction domains, assumed to be √2 × 2√2 R45, were clearly visible by this method. The reconstruction precedes the nucleation of Cu2O islands. When Cu2O islands were partially reduced and then re-oxidized, a dwell time before formation of Cu2O was noted, demonstrating that a reconstructed Cu-O surface monolayer is necessary before oxide formation.

Heteroepitaxy: The Missing Link Between Surface Chemistry and Dry Corrosion

2000 ◽  
Vol 619 ◽  
Author(s):  
Judith C. Yang ◽  
Mridula Dixit Bharadwaj ◽  
Lori Tropia
Keyword(s):  
Electron Microscopy ◽  
Water Vapor ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Solid State Reactions ◽  
Transmission Electron ◽  
Oxygen Gas ◽  
Cu Oxidation

ABSTRACTWe have investigated the initial stages of Cu (001) oxidation in dry and moist oxidizing conditions using in situ ultra-high vacuum (UIHV) transmission electron microscopy (TEM). To investigate the role of moisture in the solid state reactions in Cu oxidation, we have examined the oxidation of Cu (001) with water vapor. Our observation indicate that water vapor causes reduction of Cu2O and retards the oxidation rate if both oxygen gas and water vapor are used simultaneously which contradicts the thermochemical data. We are also modeling the nucleation to coalescence of the oxide scale using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation and have noted a qualitative agreement.

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.

In-Situ Transmission Electron Microscopy of the Formation of Metal-Semiconductor Contacts

1990 ◽  
Vol 181 ◽  
Author(s):  
J. M. Gibson ◽  
D. Loretto ◽  
D. Cherns
Keyword(s):  
High Surface ◽  
High Vacuum ◽  
Volume Ratio ◽  
Ultra High Vacuum ◽  
Silicon Surfaces ◽  
Transmission Electron ◽  
Metal Silicides ◽  
Phase Sequence ◽  
Semiconductor Contacts

ABSTRACTWe have studied the formation of metal silicides in-situ in an ultra-high vacuum transmission electron microscope. Metals were deposited on in-situ cleaned, reconstructed silicon surfaces and annealed. For the metals Ni and Co, we find that the phase sequence in ultra-thin films is different from that seen in ≈1000 Å thick films, and attribute this to the high surface-to-volume ratio. In general reactions occur at room temperature, to form an epitaxial phase if possible. We report preliminary new results on the formation of Pd2Si.

Oxidation Kinetics of Cu-Ni Alloy Observed by in situ UHV-TEM

2007 ◽  
Vol 1026 ◽  
Author(s):  
Li Sun ◽  
John E. Pearson ◽  
Judith C. Yang
Keyword(s):  
High Vacuum ◽  
Alloy Film ◽  
Ultra High Vacuum ◽  
Cross Sectional ◽  
Primary Mechanism ◽  
Transmission Electron ◽  
Ni Alloy ◽  
Cu Oxidation ◽  
Kinetics Of

AbstractThe nucleation and growth of Cu2O and NiO islands due to oxidation of Cu-24%Ni(001) films were monitored at various temperatures by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands were observed to form with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. Similar to Cu oxidation, the cross-sectional area growth rate of the oxide island is linear indicating oxygen surface diffusion is the primary mechanism of oxide growth.

In-Situ UHV TEM Investigations of the Initial Stages of Cu(001) Oxidation

1997 ◽  
Vol 3 (S2) ◽  
pp. 583-584
Author(s):  
J. C. Yang ◽  
M. Yeadon ◽  
B. Kolasa ◽  
J. M. Gibson
Keyword(s):  
High Vacuum ◽  
Copper Film ◽  
Ultra High Vacuum ◽  
Native Oxide ◽  
In Situ Tem ◽  
Face Centered Cubic ◽  
Free Standing ◽  
Transmission Electron ◽  
Face Centered

We studied the beginning oxidation stage of a model metal system by in-situ transmission electron microscopy (TEM) in order to gain insights into the initial kinetics of oxidation. In-situ TEM experiments can distinguish between nucleation and growth since individual oxide islands are imaged. We chose to investigate Cu, since it is a simple face-centered cubic metal. Also, Cu is a highly promising metal interconnect material because of its low resistivity and good electromigration properties as compared to Al.Single crystal -1000Å 99.999% purity copper films were grown on irradiated NaCl in an UHV e-beam evaporator system. The free-standing copper film was placed on a specially designed holder, which permits resistive heating of the sample. The microscope used for this experiment is a modified ultra-high vacuum, with base pressure of 10−9 torr, JEOL200CX, operated at l00kV. To remove the native oxide formed during exposure in air, the Cu film was annealed at ∼350°C

In Situ Electron Microscopy Studies of Surface Dynamical Processes

1998 ◽  
Vol 4 (S2) ◽  
pp. 608-609
Author(s):  
Ruud M. Tromp
Keyword(s):  
Electron Microscopy ◽  
Strain Relaxation ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Relaxation Phase ◽  
Transmission Electron ◽  
In Situ Electron Microscopy ◽  
Low Energy Electron ◽  
New Machine

To obtain a full and detailed understanding of the spatiotemporal dynamics of surface processes such as epitaxial growth, strain relaxation, phase transformations and phase transitions, chemisorption and etching, in situ real-time observations have proven to be invaluable. The development of two experimental techniques, i.e. Low Energy Electron Microscopy (LEEM) typically operating at electron energies below 10 eV, and Ultra-High-Vacuum Transmission Electron Microscopy (UHV-TEM) at several 100 keV, has made such in situ studies routinely possible. In many cases, the videodata obtained from such experiments are amenable to detailed, quantitative analysis, yielding statistical, kinetic and thermodynamic information that cannot be obtained in any other way.I will discuss recent experimental developments, including the design and construction of a new and improved LEEM instrument. Figure 1 shows a schematic diagram of this new machine. There are several features that distinguishes this design from most other LEEMs. One is the use of a 90 degree deflection magnetic prism array,

scholarly journals Surface Kinetics of Copper Oxidation Investigated by In Situ Ultra-high Vacuum Transmission Electron Microscopy

2001 ◽  
Vol 7 (6) ◽  
pp. 486-493 ◽  
Author(s):  
Judith C. Yang ◽  
Mridula D. Bharadwaj ◽  
Guangwen Zhou ◽  
Lori Tropia
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Water Vapor ◽  
High Vacuum ◽  
Quantitative Model ◽  
Ultra High Vacuum ◽  
Copper Oxidation ◽  
Initial Oxidation ◽  
Transmission Electron

AbstractWe review our studies of the initial oxidation stages of Cu(001) thin films as investigated by in situ ultra-high vacuum transmission electron microscopy. We present our observations of surface reconstruction and the nucleation to coalescence of copper oxide during in situ oxidation in O2. We have proposed a semi-quantitative model, where oxygen surface diffusion is the dominant mechanism of the initial oxidation stages of Cu. We have also investigated the effect of water vapor on copper oxidation. We have observed that the presence of water vapor in the oxidizing atmosphere retards the rate of Cu oxidation and Cu2O is reduced when exposed directly to steam.

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