Anomalous peaks in grazing incidence thin film X-ray diffraction

1994 ◽  
Vol 9 (1) ◽  
pp. 44-49 ◽  
Author(s):  
Richard A. Vaia ◽  
Maura S. Weathers ◽  
William A. Bassett
Keyword(s):  
Thin Films ◽  
Incidence Angle ◽  
Incident Angle ◽  
Grazing Incidence ◽  
Sample Surface ◽  
X Ray ◽  
Polymeric Thin Films ◽  
Diffraction Geometry ◽  
Sample Orientation ◽  
Diffuse Surface

Numerous spurious X-ray peaks were encountered during grazing incidence angle diffractometer scans of ceramic and polymeric thin films on crystalline and amorphous substrate materials. At least three possible sources of spurious peaks are identified. (1) At (2θ) values greater than ∼ 10°, Laue reflections from characteristic and Bremsstrahlung continuum radiation produce spurious peaks with a (2θ) dependence on X-ray incident angle and sample orientation. At (2θ) values less than 10°, (2) specular X-ray reflection from a boundary between two media of different indices of refraction and (3) diffuse surface scattering produces spurious peaks with a dependence on X-ray incident angle and sample surface topography. From an understanding of the spurious peaks, improved experimental techniques may be developed. Because these peaks can interfere significantly with grazing incidence diffractometer scans, it is particularly important to those making studies of thin films by this asymmetric diffraction geometry to be aware of the existence and origins of these spurious peaks.

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.

Design and Analysis of Hard X-Ray Microscope Employing Toroidal Mirrors Working at Grazing-Incidence

2019 ◽  
Vol 34 (04) ◽  
pp. 2055010
Author(s):  
Ying Cui ◽  
Yadong Yan ◽  
Bingjing Wu ◽  
Qi Li ◽  
Junhua He
Keyword(s):  
Optical Axis ◽  
Incidence Angle ◽  
Incident Angle ◽  
Optical Design ◽  
Grazing Incidence ◽  
Imaging Diagnosis ◽  
X Ray ◽  
Imaging Characteristics ◽  
Axis Offset ◽  
Better Than

A high resolution microscope is designed for plasma hard X-ray (10–20[Formula: see text]keV) imaging diagnosis. This system consists of two toroidal mirrors, which are nearly parallel, with an angle twice that of the grazing incidence angle and a plane mirror for spectral selection and correction of optical axis offset. The imaging characteristics of single toroidal mirror and double mirrors are analyzed in detail by the optical path function. The optical design, parameter optimization, image quality simulation and analysis of the microscope are carried out. The optimized hard X-ray microscope has a resolution better than 5[Formula: see text][Formula: see text]m at 1[Formula: see text]mm object field of view. The experimental data shows that the variation of the resolution is smaller in the direction of incident angle decrease than that in the increasing direction.

Analysis of Surface Layers and Thin Films by Low Incident Angle X-Ray Diffraction

1986 ◽  
Vol 30 ◽  
pp. 457-464 ◽  
Author(s):  
S. S. Iyengar ◽  
M. W. Santana ◽  
H. Windischmann ◽  
P. Engler
Keyword(s):  
Thin Films ◽  
Incident Angle ◽  
Grazing Incidence ◽  
Electronics Industry ◽  
Solid Surfaces ◽  
X Ray Diffraction ◽  
Surface Layers ◽  
Double Crystal ◽  
X Ray ◽  
Grazing Incidence Diffraction

Due to the current high interest in characterizing epitaxially deposited thin films required by the electronics industry as well as the increased attention in elucidating reactions between solid surfaces and the environment (e.g., corrosion), investigators have increased their efforts in developing X-ray procedures for analyzing films and surfaces less than 2 μm thick. For example, an entire session of the 1985 Denver Conference on Applications of X-ray Analysis was devoted to this subject and an excellent review of X-ray diffraction techniques for characterizing thin films was recently published by Segmuller (1). Specific techniques include grazing incidence diffraction (2, 3), double crystal diffraction (3), and the use of the Seemann-Bohlin focusing geometry (4, 5).

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.

New approach to stress analysis based on grazing-incidence X-ray diffraction

2001 ◽  
Vol 34 (4) ◽  
pp. 427-435 ◽  
Author(s):  
S. J. Skrzypek ◽  
A. Baczmański ◽  
W. Ratuszek ◽  
E. Kusior
Keyword(s):  
Residual Stresses ◽  
Grazing Incidence ◽  
Sample Surface ◽  
X Ray Diffraction ◽  
Surface Layers ◽  
Near Surface ◽  
X Ray ◽  
Tin Coatings ◽  
Diffraction Geometry ◽  
Destructive Measurement

A new development in the determination of residual stresses in thin surface layers and coatings is presented. The procedure, based on the grazing-incidence X-ray diffraction geometry (referred to here as the `g-sin2 ψ' geometry), enables non-destructive measurement at a chosen depth below the sample surface. The penetration depth of the X-ray radiation is well defined and does not change during the experiment. The method is particularly useful for the analysis of non-uniform stresses in near-surface layers. The g-sin2 ψ geometry was applied for measurements of the residual stresses in TiN coatings. Anisotropic diffraction elastic constants of textured material were used to determine the stress value from the measured lattice strains. A new method of data treatment enables reference-free measurements of residual stresses.

Growth of nano-dots on the grazing-incidence mirror surface under FEL irradiation

2016 ◽  
Vol 23 (1) ◽  
pp. 78-90 ◽  
Author(s):  
I. V. Kozhevnikov ◽  
A. V. Buzmakov ◽  
F. Siewert ◽  
K. Tiedtke ◽  
M. Störmer ◽  
...  
Keyword(s):  
Incidence Angle ◽  
Incident Angle ◽  
Grazing Incidence ◽  
Mirror Surface ◽  
Model Calculations ◽  
X Ray ◽  
Peak Intensity ◽  
Reflection Angle ◽  
Hydrocarbon Molecules ◽  
Total Disappearance

A new phenomenon on X-ray optics surfaces has been observed: the growth of nano-dots (40–55 nm diameter, 8–13 nm height, 9.4 dots µm−2surface density) on the grazing-incidence mirror surface under irradiation by the free-electron laser (FEL) FLASH (5–45 nm wavelength, 3° grazing-incidence angle). With a model calculation it is shown that these nano-dots may occur during the growth of a contamination layer due to polymerization of incoming hydrocarbon molecules. The crucial factors responsible for the growth of nano-dots in the model are the incident peak intensity and the reflection angle of the beam. A reduction of the peak intensity (e.g.replacement of the FEL beam by synchrotron radiation) as well as a decrease of the incident angle by just 1° (from 3° to 2°) may result in the total disappearance of the nano-dots. The model calculations are compared with surface analysis of two FLASH mirrors.

Thermal Expansion of Low Dielectric Constant Thin Films by High-Resolution X-Ray Reflectivity

2005 ◽  
Vol 875 ◽  
Author(s):  
Kazuhiko Omote ◽  
Yoshiyasu Ito
Keyword(s):  
Thin Films ◽  
Thermal Expansion ◽  
Incident Angle ◽  
Sample Surface ◽  
X Ray ◽  
Low Dielectric ◽  
Alignment Technique ◽  
Small Change ◽  
Sample Alignment ◽  
Low K

AbstractBy introducing high precision sample alignment technique, repeatability of incident angle to the sample surface for x-ray reflectivity (XRR) measurement is achieved to be within 0.3 arcsec. As a result, film thickness and density are possible to be measured repeatability within 0.03% and density within 0.26%. This accuracy realized to detect very small change of thermal expansion of thin films. The coefficient of thermal expansions (CTE) for porous low-k films deposited by CVD method were measured up to 400°C. The obtained values are in the range from 40 to 80 x10-6 K-1 and they are very large compare to that of copper (16-20 x10-6 K-1).

Corrections for Residual Stress in X- Ray Grazing Incidence Technique

2008 ◽  
Vol 571-572 ◽  
pp. 289-294 ◽  
Author(s):  
Sebastian Wroński ◽  
Krzysztof Wierzbanowski ◽  
Andrzej Baczmanski ◽  
Chedly Braham ◽  
Alain Lodini
Keyword(s):  
Incidence Angle ◽  
Wave Length ◽  
Grazing Incidence ◽  
Sample Surface ◽  
Peak Position ◽  
Ferrite Powder ◽  
X Ray ◽  
Wave Refraction ◽  
Small Incidence ◽  
Α Angle

Grazing incidence technique can be used to study samples with important stress gradients. The stress can be measured at very small depths, of the order of a few μm. The penetration depth of radiation is almost constant in a wide 2θ range for a given incidence angle α. It can be changed by an appropriate selection of α angle. This enables the investigation of stress variation with depth below the sample surface. There are, however, some factors which have to be corrected in this technique. The most important one is the X-ray wave refraction: it changes the wave length and direction of the beam inside a sample. These two effects cause some shift of a peak position and they have to be taken into account. For small incidence angles (α≤100) the corrections are significant and can modify the measured stress even of 70 MPa. The refraction correction decreases with increasing of the incidence angle. The corrections were tested on ferrite powder and on the ground AISI316L steel samples.

Evolution of short-range order in chemically and physically grown thin film bilayer structures for electronic applications

Nanoscale ◽  
2020 ◽  
Vol 12 (24) ◽  
pp. 13103-13112
Author(s):  
Ann-Christin Dippel ◽  
Olof Gutowski ◽  
Lars Klemeyer ◽  
Ulrich Boettger ◽  
Fenja Berg ◽  
...  
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Short Range ◽  
Short Range Order ◽  
Incidence Angle ◽  
Grazing Incidence ◽  
Distribution Functions ◽  
Individual Layer ◽  
X Ray ◽  
Pair Distribution Functions

The local atomic structure of two stacked thin films is probed by applying grazing incidence x-ray total scattering at variable incidence angle and resolving pair distribution functions for each individual layer.

Characterization of Ferroelectric PZT Thin Films - Line Broadening Study (Using Grazing Incidence Geometry)

1991 ◽  
Vol 35 (A) ◽  
pp. 601-605
Author(s):  
Michael O. Eatough ◽  
Raymond P. Goehner ◽  
Thomas J. Headley ◽  
Bruce A. Tuttle
Keyword(s):  
Thin Films ◽  
Crystallite Size ◽  
Incidence Angle ◽  
Incident Angle ◽  
Grazing Incidence ◽  
Processing Parameters ◽  
Phase Changes ◽  
Incidence Geometry ◽  
Line Broadening

AbstractFerroelectric polycrystalline thin films are being pursued as materials for use in the next generation of radiation hardened nonvolatile semiconductor memories, optical switches and optical computers. Of particular interest are PZT films with a composition near the morphotropic phase boundary. In order to fully understand the the difference in electrical properties as a function of processing parameters it is necessary to fully characterize phase composition and crystallographic properties of these films. Since some films are produced by either spinning or dipping successive layers to obtain the desired thickness it was necessary to compare the properties of each layer.X-ray diffraction techniques employing parallel beam optics with grazing incidence angle geometry were used to characterize the films. Experimental procedures using sealed tube xray diffraction systems to determine differences in crystallite size and microstrain as a function of depth into the films are a rather unique application of this technique. Discerning the contribution to line broadening due to phase changes, grazing incident angle geometry, crystallite size and microstrain are key to the success of this technique.This paper discusses the experimental techniques employed and will demonstrate how we were able to successfully determine microstrain as a function of depth into the film. We use transmission electron microscopy (TEM) to aid in the characterization of the films. A brief description of the processing procedures used to produce the films is also provided.

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