Grazing incidence synchrotron x-ray diffraction method for analyzing thin films

1987 ◽  
Vol 2 (4) ◽  
pp. 471-477 ◽  
Author(s):  
G. Lim ◽  
W. Parrish ◽  
C. Ortiz ◽  
M. Bellotto ◽  
M. Hart
Keyword(s):  
Thin Films ◽  
Penetration Depth ◽  
Incidence Angle ◽  
Depth Profiling ◽  
Diffraction Method ◽  
Grazing Incidence ◽  
Parallel Beam ◽  
X Ray ◽  
Small Incidence ◽  
Iron Oxide Films

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.

X-ray depth profiling of iron oxide thin films

1988 ◽  
Vol 3 (2) ◽  
pp. 351-356 ◽  
Author(s):  
Michael F. Toney ◽  
Ting C. Huang ◽  
Sean Brennan ◽  
Zophia Rek
Keyword(s):  
Incidence Angle ◽  
Depth Profiling ◽  
Grazing Incidence ◽  
Outward Diffusion ◽  
X Ray ◽  
X Ray Scattering ◽  
Α Phase ◽  
Small Incidence ◽  
Pattern Characteristic ◽  
Fe Ions

A nominally γ-Fe2O3 thin film (oxidized from an Fe3O4 film) has been structurally depth profiled using x-ray scattering in a grazing incidence, asymmetric Bragg geometry. By varying the grazing incidence angle, the x-ray penetration depth is varied from tens of Angstroms to several thousand Angstroms, slightly larger than the film thickness. At small incidence angles a diffraction pattern characteristic of α-Fe2O3 is observed, while at larger angles the pattern is predominantly from γ-Fe2O3, showing that there is a surface layer of α-Fe2O3. These results are quantified and the thickness of the α phase found to be 90 Å. The presence of the α phase explains a nonferromagnetic layer observed previously. These data together with magnetic and chemical data suggest that the nonferromagnetic layer forms during oxidation of the Fe3O4 film due to outward diffusion of Fe ions and their subsequent oxidation to form α-Fe2O3

Grazing-incidence X-Ray Analysis of Surfaces and Thin Films

1991 ◽  
Vol 35 (A) ◽  
pp. 143-150 ◽  
Author(s):  
T. C. Huang
Keyword(s):  
Thin Films ◽  
Depth Profiling ◽  
Grazing Incidence ◽  
Bragg Diffraction ◽  
Interface Roughness ◽  
Phase Identification ◽  
X Ray ◽  
Types Of Information

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.

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
Keyword(s):  
Thin Films ◽  
Heat Treatment ◽  
Profile Analysis ◽  
Protective Coatings ◽  
Depth Profiling ◽  
Grazing Incidence ◽  
Metallic Thin Films ◽  
X Ray ◽  
Secondary Ions ◽  
The Stability

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.

scholarly journals Déposition par Pulvé Risation Cathodique Radio Fréquence et Caracté Risation Électronique, Structurale et Optique de Couches Minces du Dioxyde de Titane

2004 ◽  
Vol 27 (3) ◽  
pp. 169-181 ◽  
Author(s):  
K. Hafidi ◽  
M. Azizan ◽  
Y. Ijdiyaou ◽  
E. L. Ameziane
Keyword(s):  
Thin Films ◽  
Titanium Oxide ◽  
Incidence Angle ◽  
Glass Structure ◽  
Grazing Incidence ◽  
Visible Range ◽  
Infrared Range ◽  
Oxide Thin Films ◽  
X Ray ◽  
Deposited Films

Deposited titanium oxide thin films are used as optical protector films for several materials and as energy converters for solar cells. In this work, titanium oxide thin films are deposited on c-Si and glass substrates by reactive radiofrequency sputtering. All the deposits are grown at ambient temperature and the sputtering gas is a mixture of oxygen and argon with an overall pressure of10−2mbar. The oxygen partial pressure ratios varies from 5% to 20%.Characterization of deposited films is made by grazing incidence X-ray diffraction (GIXD), grazing incidence X-ray reflection (GIXR), X-ray photoemission spectroscopy (XPS) and optical transmission spectroscopy. The characterization results reveal that deposited films of TiO2 are polycrystalline and present both rutile and anatase phases. The chemical composition of raw films in Ti:O ratio is equal to 1:2.02, and the titanium at surface is completely oxidized. In fact, the Ti2p core level behavior shows that the oxidization state of Ti is equal to+4.The specularily reflected intensity according to incidence angle of the X-ray on TiO2/glass structure shows one critical angle attributed to the TiO2 film equal to 0.283º. This angle value involves film density between rutile and anatase phases. The optical characterization shows that TiO2 thin films obtained are transparent in visible range, and have a refraction index value equal to 2.45 and when extrapolated to infrared range, it is equal to 2.23. The value of gap energy (3.35 eV) is deduced from variation of absorption coefficient versus incident radiation energy.

Effects of Refraction and Reflection on Analysis of Thin Films by the Grazing-Incidence X-ray Diffraction Method

1989 ◽  
Vol 33 ◽  
pp. 109-120 ◽  
Author(s):  
Toru Takayama ◽  
Yoshiro Matsumoto
Keyword(s):  
Thin Films ◽  
Room Temperature ◽  
Diffraction Method ◽  
Grazing Incidence ◽  
X Ray Diffraction ◽  
Diffraction Intensity ◽  
X Ray ◽  
Evaporation Technique ◽  
Diffraction Peaks ◽  
Angular Shift

AbstractThe grazing-incidence X-ray diffraction (GIXD) method was employed to analyze two-layer thin films, which were the samples of Å lOO Å Au/500Å Cu/Si02(substrate) and 250Å Cu/500Å Au/SiO2(substrate), which were prepared by the evaporation technique under the condition that the SiO2substrate was at room temperature. Diffraction profiles were obtained at various glancing angles ( α ) and the data were analyzed as a function of α. The results were as follows : 1) Diffraction peaks were shifted to larger diffraction angles, because of the refraction of the incident X-ray beam. The angular shift has been approximated by the equation, α - α2- αc2)1/2, where αcis the total ref reflection critical angle of the material. 2) As a result of the correction of angular shift, the stress of the evaporated films was estimated to be null. 3) The broadening of the Cu diffraction peak and the enhancement of the Cu diffraction intensity occurred at angles near αcof Cu, due to the reflection of the X-ray beam at the Cu/Au interface.

scholarly journals Interface-sensitive imaging by an image reconstruction aided X-ray reflectivity technique

2017 ◽  
Vol 50 (3) ◽  
pp. 712-721 ◽  
Author(s):  
Jinxing Jiang ◽  
Keiichi Hirano ◽  
Kenji Sakurai
Keyword(s):  
Ultrathin Films ◽  
Incidence Angle ◽  
Grazing Incidence ◽  
Two Dimensional ◽  
Plane Angle ◽  
Pixel Size ◽  
Parallel Beam ◽  
X Ray ◽  
Area Detector ◽  
Grazing Incidence Angle

Recently, the authors have succeeded in realizing X-ray reflectivity imaging of heterogeneous ultrathin films at specific wavevector transfers by applying a wide parallel beam and an area detector. By combining in-plane angle and grazing-incidence angle scans, it is possible to reconstruct a series of interface-sensitive X-ray reflectivity images at different grazing-incidence angles (proportional to wavevector transfers). The physical meaning of a reconstructed X-ray reflectivity image at a specific wavevector transfer is the two-dimensional reflectivity distribution of the sample. In this manner, it is possible to retrieve the micro-X-ray reflectivity (where the pixel size is on the microscale) profiles at different local positions on the sample.

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