The Surface Kinetics of the Initial Oxidation Stages of Cu and Cu Alloys
Judith C. Yang,* Yihong Kang,* Langli Luo,** Chris Fleck,* Minyoung Lee,*** Jeffrey A.
Eastman,**** Alan McGaughey*** and Guangwen Zhou**
* Department of Mechanical Engineering and Materials Science, University of Pittsburgh,
Pittsburgh, PA 15261
** Department of Mechanical Engineering, State University of New York, Binghamton, NY13902
*** Department of Mechanical Engineering, Carnegie Mellon University, Pittsburgh, PA 15213
**** Materials Science Division, Argonne National Laboratory, Argonne, IL, 60439
Environmental stability is one of the most important properties for materials exposed to air. As the
dimensions of engineered systems approach the nanoscale, fundamental understanding of reactions
with oxygen at this length scale becomes critical for environmental stability as well as for processing
oxide nanostructures, where surface reactions are commonly used. Because environmental stability
is an essential property of most engineered materials, many theories exist to explain oxidation and
corrosion mechanisms. However, nearly all classical oxidation theories assume a uniform growing
film, where structural changes are not considered because of the previous lack of experimental
procedures to visualize non-uniform growth conditions. These macroscopic depictions do not
address how initial surface conditions and early stages of oxidation lead to the final oxide scale
morphology, though it is well known that surface conditions and secondary elements dramatically
impact the oxide structure. These transient stages of oxidation — from the nucleation of the metal
oxide to the formation of the thermodynamically stable oxide — represent a scientifically
challenging and technologically important terra incognito.
These issues can only be understood through detailed structural study of the relevant microscopic
processes at the nanoscale in situ, combined with comparison to theoretical models. Hence, we are
studying the dynamics of the initial and transient oxidation stages of a metal and its alloys with in
situ methods, including ultra-high vacuum transmission electron microscopy (UHV-TEM) and
synchrotron X-ray diffraction. We examined the dynamic responses of Cu and Cu alloy thin films to
variations in thermodynamic variables such as temperature, oxygen partial pressure (pO
2
), strain,
and crystallographic orientation. Our past work demonstrated that the formation of epitaxial Cu
2
O
islands during the transient oxidation of Cu(100), (110) and (111) films bears a striking resemblance
to heteroepitaxy, where the initial stages of growth are dominated by oxygen surface diffusion and
strain impacts the evolution of the oxide morphologies [1-4]. We are currently developing multi-
scale simulations to directly compare to the Cu oxidation data and provide insight into the
mechanisms controlling the initial stages of oxidation [5]. For example, a kinetic Monte Carlo code
has been developed to describe three-dimensional island nucleation and growth (www.tfox.org ) [6].
The kinetics of early stage oxidation of Cu, Cu-Au and Cu-Ni alloys were visualized using in situ
ultra-high vacuum transmission electron microscopy (UHV-TEM), where the initial oxidation stages
can be observed in real-time under well-controlled surface conditions. These experiments were
carried out in a modified JEOL 200CX TEM. This microscope is equipped with an ultra-high
vacuum (UHV) chamber with base pressure ~ 10
-8
Torr. The microscope was operated at 100KeV to
minimize the possibility of radiation-induced effects. A controlled leak valve attached to the column
permits the introduction of oxygen gas directly into the microscope at a pO
2
between 5×10
-5
and
1406
doi:10.1017/S143192761005453X
Microsc. Microanal. 16 (Suppl 2), 2010
© Microscopy Society of America 2010
https://doi.org/10.1017/S143192761005453X Published online by Cambridge University Press