Investigation of Thin Coatings from Mn-Co-Fe System Deposited by PVD on Metallic Interconnects for SOFC Applications

2008 ◽  
Vol 595-598 ◽  
pp. 797-804 ◽  
Author(s):  
Cezarina C. Mardare ◽  
Michael Spiegel ◽  
Alan Savan ◽  
Alfred Ludwig

Ternary Mn-Co-Fe metallic thin films were deposited by RF-magnetron co-sputtering on SiO2/Si wafers and on ZMG232L (Hitachi Metals®), a special ferritic stainless steel for Solid Oxide Fuel Cell applications. The deposition was followed by heat treatment in an oxidizing atmosphere in order to convert the metallic thin films to (Mn,Co,Fe)3O4 spinel oxides. Coated and uncoated steel samples were analyzed after 1 h heat treatment in order to confirm the presence of the spinel structure on top of the steel, as well as to investigate and characterize the growth of oxides, namely (Mn,Cr)3O4 and Cr2O3, at the internal steel/coating interface. From Grazing Incidence X-ray Diffraction (GI-XRD) investigations together with Energy Dispersive X-ray analysis – Scanning Electron Microscopy and Time of Flight – Secondary Ions Mass Spectroscopy sputtering depth profiling the presence of well adherent (Mn,Co,Fe)3O4 coatings with approximately 500 nm thickness and a grain size of about 150 nm was confirmed. After the preparation annealing, some samples were heat-treated in simulated cathodic atmospheres at 800 °C for 500 h in order to assess the stability of the coatings. GI-XRD spectra still showed the presence of the protective coatings, however sputtering depth profile analysis indicated the presence of Cr on the surface.

1991 ◽  
Vol 35 (A) ◽  
pp. 143-150 ◽  
Author(s):  
T. C. Huang

AbstractGrazing-incidence X-ray analysis techniques which are commonly used for the nondestructive characterization of surfaces and thin films are reviewed. The X-ray reflectivity technicue is used to study surface uniformity and oxidation, layer thickness and density, interface roughness and diffusion, etc. The grazing-incidence in-plane diffraction technique is used to determine in-plane crystallography of epitaxial films. The grazing-incidence asymmetric-Bragg diffraction is used for surface phase identification and structural depth profiling determination of polycrystalline films. Typical examples to illustrate the types of information that can be obtained by the techniques are presented.


1987 ◽  
Vol 2 (4) ◽  
pp. 471-477 ◽  
Author(s):  
G. Lim ◽  
W. Parrish ◽  
C. Ortiz ◽  
M. Bellotto ◽  
M. Hart

A method using synchrotron radiation parallel beam x-ray optics with a small incidence angle α on the specimen and 2Θ-detector scanning is described for depth profiling analysis of thin films. The instrumentation is the same as used for Θ:2Θ synchrotron parallel beam powder diffractometry, except that the specimen is uncoupled from the detector. There is no profile distortion. Below the critical angle for total reflection αc, the top tens of Angstroms are sampled. Depth profiling is controlled to a few Angstroms using a small α and 0.005° steps. The penetration depth increases to several hundred Angstroms as α approaches αc. Above αc there is a rapid increase in penetration depth to a thousand Angstroms or more and the profiling cannot be sensitively controlled. At grazing incidence the peaks are shifted several tenths of a degree by the x-ray refraction and an experimental procedure for calculating the shifts is described. The method is illustrated with an analysis of iron oxide films.


1991 ◽  
Vol 35 (B) ◽  
pp. 807-812
Author(s):  
Hideki Hashimoto ◽  
Hiroshi Nishioji ◽  
Hideo Saisho

AbstractReflection and fluorescence intensity profile curves for thin films were measured under the grazing incidence conditions using synchrotron radiation. A titanium layer and a carbon / titanium bilayer sputtered on a silicon wafer were subjected to heat treatment. The analysis of the reflection and fluorescence profile curves shows that the sample without the heat treatment has another high-density layer on the surface or interface, and that the heat treatment results in the removal of the high-density layer and the formation of a thick homogeneous layer.


2009 ◽  
Vol 42 (6) ◽  
pp. 1158-1164 ◽  
Author(s):  
Narcizo M. Souza-Neto ◽  
Aline Y. Ramos ◽  
Hélio C. N. Tolentino ◽  
Alessandro Martins ◽  
Antonio D. Santos

A method of using X-ray absorption spectroscopy together with resolved grazing-incidence geometry for depth profiling of atomic, electronic or chemical local structures in thin films is presented. The quantitative deconvolution of thickness-dependent spectral features is performed by fully considering both scattering and absorption formalisms. Surface oxidation and local structural depth profiles in nanometric FePt films are determined, exemplifying the application of the method.


2003 ◽  
Vol 18 (1) ◽  
pp. 173-179 ◽  
Author(s):  
Maxim B. Kelman ◽  
Paul C. McIntyre ◽  
Bryan C. Hendrix ◽  
Steven M. Bilodeau ◽  
Jeffrey F. Roeder ◽  
...  

Structural properties of polycrystalline Pb(Zr0.35Ti0.65)O3 (PZT) thin films grown by metalorganic chemical vapor deposition on Ir bottom electrodes were investigated. Symmetric x-ray diffraction measurements showed that as-deposited 1500 íthick PZT films are partially tetragonal and partially rhombohedral. Cross-section scanning electron microscopy showed that these films have a polycrystalline columnar microstructure with grains extending through the thickness of the film. X-ray depth profiling using the grazing-incidence asymmetric Bragg scattering geometry suggests that each grain has a bilayer structure consisting of a near-surface region in the etragonal phase and the region at the bottom electrode interface in the rhombohedral hase. The required compatibility between the tetragonal and rhombohedral phases in he proposed layered structure of the 1500 Å PZT can explain the peak shifts observed n the symmetric x-ray diffraction results of thicker PZT films.


Author(s):  
R. M. Anderson

Aluminum-copper-silicon thin films have been considered as an interconnection metallurgy for integrated circuit applications. Various schemes have been proposed to incorporate small percent-ages of silicon into films that typically contain two to five percent copper. We undertook a study of the total effect of silicon on the aluminum copper film as revealed by transmission electron microscopy, scanning electron microscopy, x-ray diffraction and ion microprobe techniques as a function of the various deposition methods.X-ray investigations noted a change in solid solution concentration as a function of Si content before and after heat-treatment. The amount of solid solution in the Al increased with heat-treatment for films with ≥2% silicon and decreased for films <2% silicon.


Author(s):  
Jonathan Ogle ◽  
Daniel Powell ◽  
Eric Amerling ◽  
Detlef Matthias Smilgies ◽  
Luisa Whittaker-Brooks

<p>Thin film materials have become increasingly complex in morphological and structural design. When characterizing the structure of these films, a crucial field of study is the role that crystallite orientation plays in giving rise to unique electronic properties. It is therefore important to have a comparative tool for understanding differences in crystallite orientation within a thin film, and also the ability to compare the structural orientation between different thin films. Herein, we designed a new method dubbed the mosaicity factor (MF) to quantify crystallite orientation in thin films using grazing incidence wide-angle X-ray scattering (GIWAXS) patterns. This method for quantifying the orientation of thin films overcomes many limitations inherent in previous approaches such as noise sensitivity, the ability to compare orientation distributions along different axes, and the ability to quantify multiple crystallite orientations observed within the same Miller index. Following the presentation of MF, we proceed to discussing case studies to show the efficacy and range of application available for the use of MF. These studies show how using the MF approach yields quantitative orientation information for various materials assembled on a substrate.<b></b></p>


1996 ◽  
Vol 440 ◽  
Author(s):  
P. C. Chow ◽  
R. Paniago ◽  
R. Forrest ◽  
S. C. Moss ◽  
S. S. P. Parkin ◽  
...  

AbstractThe growth by sputtering of a series of thin films of Fe/Au on MgO(001) substrates was analyzed using Bragg and diffuse X-ray scattering. The Fe (bcc) layer grows rotated by 45° with respect to the MgO – Au(fcc) (001) epitaxial orientation, resulting in an almost perfect match between the two metallic structures. By collecting the X-ray diffuse scattering under grazing incidence using a 2-dimensional image plate detector, we mapped the reciprocal space of these films. We characterized the correlated interface roughness starting with a buffer of Fe in which only three interfaces are present. The propagation of the roughness was subsequently characterized for Fe/Au multilayers with 40 and 100 bilayers. We observe an enlargement of the surface features as a function of time, evidenced by the longer lateral cutoff length measured for thicker films.


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