Journal articles: 'Grazing incidence X-ray diffraction (GIXD)'

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Takagi, Yasuo, and Masao Kimura. "Generalized grazing-incidence-angle X-ray diffraction (G-GIXD) using image plates." Journal of Synchrotron Radiation 5, no. 3 (May 1, 1998): 488–90. http://dx.doi.org/10.1107/s090904959800123x.

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A new and more `generalized' grazing-incidence-angle X-ray diffraction (G-GIXD) method which enables simultaneous measurements both of in- and out-of-plane diffraction images from surface and interface structures has been developed. While the method uses grazing-incidence-angle X-rays like synchrotron radiation as an incident beam in the same manner as in `traditional' GIXD, two-dimensional (area) detectors like image plates and a spherical-type goniometer are used as the data-collection system. In this way, diffraction images both in the Seemann–Bohlin (out-of-plane) and GIXD geometry (in-plane) can be measured simultaneously without scanning the detectors. The method can be applied not only to the analysis of the in-plane crystal structure of epitaxically grown thin films, but also to more general research topics like the structural analysis of polycrystalline mixed phases of thin surface and interface layers.

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Kainz, Manuel Peter, Lukas Legenstein, Valentin Holzer, Sebastian Hofer, Martin Kaltenegger, Roland Resel, and Josef Simbrunner. "GIDInd: an automated indexing software for grazing-incidence X-ray diffraction data." Journal of Applied Crystallography 54, no. 4 (July 30, 2021): 1256–67. http://dx.doi.org/10.1107/s1600576721006609.

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Grazing-incidence X-ray diffraction (GIXD) is a widely used technique for the crystallographic characterization of thin films. The identification of a specific phase or the discovery of an unknown polymorph always requires indexing of the associated diffraction pattern. However, despite the importance of this procedure, only a few approaches have been developed so far. Recently, an advanced mathematical framework for indexing of these specific diffraction patterns has been developed. Here, the successful implementation of this framework in the form of an automated indexing software, named GIDInd, is introduced. GIDInd is based on the assumption of a triclinic unit cell with six lattice constants and a distinct contact plane parallel to the substrate surface. Two approaches are chosen: (i) using only diffraction peaks of the GIXD pattern and (ii) combining the GIXD pattern with a specular diffraction peak. In the first approach the six unknown lattice parameters have to be determined by a single fitting procedure, while in the second approach two successive fitting procedures are used with three unknown parameters each. The output unit cells are reduced cells according to approved crystallographic conventions. Unit-cell solutions are additionally numerically optimized. The computational toolkit is compiled in the form of a MATLAB executable and presented within a user-friendly graphical user interface. The program is demonstrated by application on two independent examples of thin organic films.

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Breiby, Dag W., Oliver Bunk, Jens W. Andreasen, Henrik T. Lemke, and Martin M. Nielsen. "Simulating X-ray diffraction of textured films." Journal of Applied Crystallography 41, no. 2 (March 8, 2008): 262–71. http://dx.doi.org/10.1107/s0021889808001064.

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Computationally efficient simulations of grazing-incidence X-ray diffraction (GIXD) are discussed, with particular attention given to textured thin polycrystalline films on supporting substrates. A computer program has been developed for simulating scattering from thin films exhibiting varying degrees of preferred orientation. One emphasized common case is that of a `fibre' symmetry axis perpendicular to the sample plane, resulting from crystallites having one well defined crystal facet towards the substrate, but no preferred in-plane orientation. Peak splitting caused by additional scattering from the totally substrate-reflected beam (two-beam approximation) and refraction effects are also included in the program, together with the geometrical intensity corrections associated with GIXD measurements. To achieve `user friendliness' for scientists less familiar with diffraction, the mathematically simplest possible descriptions are sought whenever feasible. The practical use of the program is demonstrated for a selected thin-film example, perylene, which is of relevance for organic electronics.

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Khasanah, Khasanah, Isao Takahashi, Kummetha Raghunatha Reddy, and Yukihiro Ozaki. "Crystallization of ultrathin poly(3-hydroxybutyrate) films in blends with small amounts of poly(l-lactic acid): correlation between film thickness and molecular weight of poly(l-lactic acid)." RSC Advances 7, no. 83 (2017): 52651–60. http://dx.doi.org/10.1039/c7ra10996b.

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The crystallization behavior of poly(3-hydroxybutyrate) (PHB) films in blends with small amounts of poly(l-lactic acids) (PLLAs) was investigated by grazing incidence X-ray diffraction (GIXD) and infrared-reflection absorption spectroscopy (IRRAS).

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Hafidi, K., M. Azizan, Y. Ijdiyaou, and E. L. Ameziane. "Ètude des interfaces SiO2/TiO2 et TiO2/SiO2 dans la structure SiO2/TiO2/SiO2/c-Si préparée par pulvérisation cathodique radio fréquence." Canadian Journal of Physics 85, no. 7 (July 1, 2007): 763–76. http://dx.doi.org/10.1139/p07-053.

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The atomic structure of the TiO2/SiO2 and SiO2/TiO2 interfaces has been investigated in SiO2/TiO2/SiO2 multilayers deposited by radio frequency reactive sputtering without breaking the vacuum on the crystalline substrate cooled by water. The characterizations of these interfaces have been performed using three complementary techniques sensitive to surface and interface state: X-ray photoelectron spectroscopy (XPS), grazing incidence X-ray diffraction (GIXD), and specular X-ray reflectometry (GIXR). The concentration profiles and Si2p and O1s core level chemical displacements show that TiO2/SiO2 and SiO2/TiO2 interfaces are very diffuse. The reflectometry measurements confirm this character and indicate that the silicon, titanium, and oxygen atomic concentrations vary gradually at the interfaces. The grazing incidence X-ray spectra indicates that the interfacial layers are not well crystallized and are formed by SiO2-TiO2, TiO, Ti2O3, Ti3O5, Ti5Si3, Ti5Si4, TiSi, and TiSi2 components.

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Ishida, Kenji, Akinori Kita, Kouichi Hayashi, Toshihisa Horiuchi, Shoichi Kal, and Kazumi Matsushige. "Energy Dispersive Grazing Incidence X-ray Diffraction Study on Organic Thin Films EpitaxiaHy Grown on Crystalline Substrate." Advances in X-ray Analysis 39 (1995): 659–64. http://dx.doi.org/10.1154/s0376030800023090.

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Thin film technology is rapidly evolving today, and the characterization of the thin film and its surface have become very important issue not only from scientific but also technological viewpoints. Although x-ray diffraction measurements have been used as suitable evaluation methods in crystallography studies, its application to the structural evaluation of the thin films, especially organic one having the low electron densities, is not easy due to the small amounts of scattering volume and the high obstructive scattering noise from the substrate. However, the x-ray diffraction measurements under grazing incidence will aid not only in overcoming the such problems but also in analyzing in-plane structure of the thin films. Therefore, so-called grazing incidence x-ray diffraction (GIXD) has been recognized as one of the most powerful tools for the surface and thin film studies.

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Gobato, Ricardo, Marcia Regina Risso Gobato, Alireza Heidari, and Abhijit Mitra. "Unrestricted hartree-fock computational simulation in a protonated rhodochrosite crystal." Physics & Astronomy International Journal 3, no. 6 (November 6, 2019): 220–28. http://dx.doi.org/10.15406/paij.2019.03.00187.

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In this paper, compact effective potentials, charge distribution, Atomic Polar Tensor (APT) and Mulliken charges were studied using a unrestricted Hartree-Fock computational simulation in a protonated rhodochrosite crystal. The rhodochrosite crystal unit cell of structure CMn6O8, where the charge distribution by the molecule was verified in the UHF CEP-4G (Effective core potential (ECP) minimal basis), UHF CEP-31G (ECP split valance) and UHF CEP-121G (ECP triple-split basis). The largest load variation in the APT and Mulliken methods were obtained in the CEP-121G basis set, with δ=2.922 e δ=2.650 u.a., respectively, being δAPT> δMulliken. The maximum absorbance peaks in the CEP-4G, CEP-31G and CEP-121G basis set are present at the frequencies 2172.23 cm-1, with a normalized intensity of 0.65; 2231.4 cm-1 and 0.454; and 2177.24 cm-1 and 1.0, respectively. An in-depth study is necessary to verify the absorption by the tumoral and non-tumoral tissues of rhodochrosite, before and after irradiating of synchrotron radiation using Small–Angle X–Ray Scattering (SAXS), Ultra–Small Angle X–Ray Scattering (USAXS), Fluctuation X–Ray Scattering (FXS), Wide–Angle X–Ray Scattering (WAXS), Grazing–Incidence Small–Angle X–Ray Scattering (GISAXS), Grazing–Incidence Wide–Angle X–Ray Scattering (GIWAXS), Small–Angle Neutron Scattering (SANS), Grazing–Incidence Small–Angle Neutron Scattering (GISANS), X–Ray Diffraction (XRD), Powder X–Ray Diffraction (PXRD), Wide–Angle X–Ray Diffraction (WAXD), Grazing– Incidence X–Ray Diffraction (GIXD) and Energy–Dispersive X–Ray Diffraction (EDXRD). Later studies could check the advantages and disadvantages of rhodochrosite in the treatment of cancer through synchrotron radiation, such as one oscillator crystal.

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Holzer, Valentin, Benedikt Schrode, Josef Simbrunner, Sebastian Hofer, Luisa Barba, Roland Resel, and Oliver Werzer. "Impact of sample misalignment on grazing incidence x-ray diffraction patterns and the resulting unit cell determination." Review of Scientific Instruments 93, no. 6 (June 1, 2022): 063906. http://dx.doi.org/10.1063/5.0088176.

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Grazing incidence x-ray diffraction (GIXD) is a frequently used tool for the crystallographic characterization of thin films in terms of polymorph identification and determination of the crystallographic lattice parameters. Even full structure solutions are possible. To obtain highly accurate diffraction patterns, the thin film sample has to be aligned carefully with the center of the goniometer, which allows a defined incidence of the primary x-ray beam relative to the sample surface. This work studies the effect of misalignment of a thin film sample on the acquired diffraction pattern. Three potential types of misalignments are considered: the deviation of the sample surface from the center of the goniometer, an error in the incidence angle of the primary beam, and an inclination of the goniometer rotation axis from the normal of the substrate surface. The consequence of these types of sample misalignments is the shift of diffraction peaks toward specific directions in reciprocal space. Mathematical equations are given that relate the error in positions of Bragg peaks for each type of sample misalignment. Experiments with intentionally misaligned samples confirm the given formulas. In a subsequent step, the errors in the peak positions are translated to systematic errors in the estimation of the unit cell parameters. Depending on the type of misalignment, some alignment errors can be reduced or even corrected; in particular, azimuthal sample rotations prove to be advantageous in these cases. The results in this work improve the quality of GIXD measurements, in general, enabling deeper analysis like the full structure solution from the GIXD pattern on everyday basis.

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Yoshida, Masahiro, Yasunori Kutsuma, Daichi Dohjima, Kenji Ohwada, Toshiya Inami, Noboru Ohtani, Tadaaki Kaneko, and Jun'ichiro Mizuki. "Development of the Compact Furnace for the In Situ Observation under Ultra-High Temperature by Synchrotron x-Ray Surface Diffraction." Materials Science Forum 858 (May 2016): 505–8. http://dx.doi.org/10.4028/www.scientific.net/msf.858.505.

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We have established the grazing-incidence x-ray diffraction (GIXD) method under ultra- high temperature for in-situ crystal growth observation. For this purpose, we have developed the compact furnace which can be mounted on a goniometer used for the GIXD experiment. Using the custom-designed furnace, we have succeeded in controlling very high temperature around 1800°C. Subsequently, we have proved the performance of the furnace through the measurement of the tem- perature dependence of a-lattice constant of 4H-SiC in the range from room temperature to 1500 °C.

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Silva, Gonçalo M. C., Pedro Morgado, Pedro Lourenço, Michel Goldmann, and Eduardo J. M. Filipe. "Spontaneous self-assembly and structure of perfluoroalkylalkane surfactant hemimicelles by molecular dynamics simulations." Proceedings of the National Academy of Sciences 116, no. 30 (July 5, 2019): 14868–73. http://dx.doi.org/10.1073/pnas.1906782116.

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Fully atomistic molecular-dynamics (MD) simulations of perfluoroalkylalkane molecules at the surface of water show the spontaneous formation of aggregates whose size and topography closely resemble the experimentally observed hemimicelles for this system. Furthermore, the grazing incidence X-ray diffraction (GIXD) pattern calculated from the simulation trajectories reproduces the experimental GIXD spectra previously obtained, fully validating the MD simulation results. The detailed analysis of the internal structure of the aggregates obtained by the MD simulations supports a definite rational explanation for the spontaneous formation, stability, size, and shape of perfluoroalkylalkane hemimicelles at the surface of water.

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Yazdanmehr, Amir, and Hamid Jahed. "On the Surface Residual Stress Measurement in Magnesium Alloys Using X-Ray Diffraction." Materials 13, no. 22 (November 17, 2020): 5190. http://dx.doi.org/10.3390/ma13225190.

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X-ray penetration in magnesium alloys is significant due to the low X-ray mass attenuation coefficient. To measure the surface residual stresses in magnesium alloys, a correction needs to be made to account for penetration depth. The residual stresses in as-received and shot peened AZ31B-H24 rolled sheet samples were measured using two-dimensional X-ray diffraction (2D-XRD) method. The electro-polishing layer removal method was used to find the residual stress pattern at the surface and through the depth. The results show that the corrected residual stresses in a few tens of micrometers layer from the surface differ from the raw stresses. To better estimate the residual stress distribution in the surface, the grazing-incidence X-ray diffraction (GIXD) technique was applied. Additionally, micrographs of the lateral cross-section of the peened specimens confirmed the presence of microcracks in this region, causing the residual stresses to vanish. Due to the low X-ray absorption coefficient of Mg alloys, this study shows how a small uncertainty in a single raw measurement leads to high uncertainty in the corrected residual stresses. The results were corroborated with the hole drilling method of residual stress measurements. The corrected X-ray diffraction (XRD) results are in close agreement with the hole drilling and GIXD results.

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Cyboroń, Jolanta. "Residual stress analysis after machining in composite materials based on aluminum alloy with ceramic additive." Mechanik 91, no. 1 (January 8, 2018): 28–30. http://dx.doi.org/10.17814/mechanik.2018.1.4.

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The paper presents the results of structural studies of AlSi7Mg alloy with 5% vol. addition of silicon carbide (SiC), after the machining process using the alternative method including: electrical discharge machining (EDM), abrasive water jet (AWJ) and cutting. The article presents the possibilities of measuring the impact of selected machining techniques on the surface and subsurface layers. X-ray diffraction were used to determine the level and characters of the obtained residual stresses. The article presents the X-ray diffraction method in the grazing incidence X-ray diffraction technique (GIXD) used for the practical measurement of the range of changes within the surface layer formed, as a result of interaction between the tool and the surface of the material being processed.

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Tanigaki, Nobutaka, Chikayo Takechi, Shuichi Nagamatsu, Toshiko Mizokuro, and Yuji Yoshida. "Oriented Thin Films of Insoluble Polythiophene Prepared by the Friction Transfer Technique." Polymers 13, no. 15 (July 21, 2021): 2393. http://dx.doi.org/10.3390/polym13152393.

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A thin film of unsubstituted polythiophene (PT), an insoluble conjugated polymer, with molecular chains uniaxially oriented in plane was prepared by the friction transfer method. The structure of highly oriented thin films of PT was investigated using grazing-incidence X-ray diffraction (GIXD), ultraviolet–visible (UV–vis) spectroscopy, and infrared (IR) spectroscopy. The polarized UV–vis and IR spectra and GIXD measurements showed the PT molecular chains were well aligned in parallel to the friction direction. The GIXD studies clarified that the polymer backbones were aligned with very narrow distribution, such that the half-width was about 4 degrees. The degree of orientation of the PT friction-transferred film was higher compared with those of regioregular poly(3-alkylthiophene)s. Moreover, the GIXD results show a preferred orientation where the a-axis is perpendicular to the substrate plane.

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Foran, Garry J., Richard F. Garrett, Ian R. Gentle, Dudley C. Creagh, Jian Bang Peng, and Geoffrey T. Barnes. "Focusing monochromator and imaging-plate camera for grazing-incidence diffraction studies of thin films." Journal of Synchrotron Radiation 5, no. 3 (May 1, 1998): 500–502. http://dx.doi.org/10.1107/s0909049597017287.

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A multiple-imaging-plate detector system and focusing monochromator have been developed and successfully applied to the time-resolved study of phase transitions in Langmuir–Blodgett films by grazing-incidence X-ray diffraction (GIXD). The monochromator described here combines fixed-exit-beam height with sagittal focusing of the second crystal. The design is similar to that of Matsushita et al. [Matsushita, Ishikawa & Oyanagi (1986). Nucl. Instrum. Methods, A246, 377–379], with the exception that the motion of the first crystal is achieved via a computer-controlled X-Y translation table rather than a set of cams. The second crystal is a ribbed Si(111) wafer mounted in a four-point bending mechanism. The first reported application of imaging plates to a GIXD study was carried out by our group and proved to be very successful in the determination of thin-film structure [Foran, Peng, Steitz, Barnes & Gentle (1996). Langmuir, 12, 774–777]. To extend the capabilities of this system, an imaging-plate camera was designed and built which can accommodate up to 13 imaging plates (40 × 20 cm) inside the vacuum chamber of the main diffractometer at the Australian Beamline at the Photon Factory.

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Simbrunner, Josef, Clemens Simbrunner, Benedikt Schrode, Christian Röthel, Natalia Bedoya-Martinez, Ingo Salzmann, and Roland Resel. "Indexing of grazing-incidence X-ray diffraction patterns: the case of fibre-textured thin films." Acta Crystallographica Section A Foundations and Advances 74, no. 4 (July 1, 2018): 373–87. http://dx.doi.org/10.1107/s2053273318006629.

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Crystal structure solutions from thin films are often performed by grazing-incidence X-ray diffraction (GIXD) experiments. In particular, on isotropic substrates the thin film crystallites grow in a fibre texture showing a well defined crystallographic plane oriented parallel to the substrate surface with random in-plane order of the microcrystallites forming the film. In the present work, analytical mathematical expressions are derived for indexing experimental diffraction patterns, a highly challenging task which hitherto mainly relied on trial-and-error approaches. The six lattice constants a, b, c, α, β and γ of the crystallographic unit cell are thereby determined, as well as the rotation parameters due to the unknown preferred orientation of the crystals with respect to the substrate surface. The mathematical analysis exploits a combination of GIXD data and information acquired by the specular X-ray diffraction. The presence of a sole specular diffraction peak series reveals fibre-textured growth with a crystallographic plane parallel to the substrate, which allows establishment of the Miller indices u, v and w as the rotation parameters. Mathematical expressions are derived which reduce the system of unknown parameters from the three- to the two-dimensional space. Thus, in the first part of the indexing routine, the integers u and v as well as the Laue indices h and k of the experimentally observed diffraction peaks are assigned by systematically varying the integer variables, and by calculating the three lattice parameters a, b and γ. Because of the symmetry of the derived equations, determining the missing parameters then becomes feasible: (i) w of the surface parallel plane, (ii) the Laue indices l of the diffraction peak and (iii) analogously the lattice constants c, α and ß. In a subsequent step, the reduced unit-cell geometry can be identified. Finally, the methodology is demonstrated by application to an example, indexing the diffraction pattern of a thin film of the organic semiconductor pentacenequinone grown on the (0001) surface of highly oriented pyrolytic graphite. The preferred orientation of the crystallites, the lattice constants of the triclinic unit cell and finally, by molecular modelling, the full crystal structure solution of the as-yet-unknown polymorph of pentacenequinone are determined.

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Takayama, Toru, and Yoshiro Matsumoto. "Effects of Refraction and Reflection on Analysis of Thin Films by the Grazing-Incidence X-ray Diffraction Method." Advances in X-ray Analysis 33 (1989): 109–20. http://dx.doi.org/10.1154/s0376030800019492.

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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.

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Chang, Chenyuan, Zhenbo Wei, Hui Jiang, Hangjian Ni, Wentao Song, Jialian He, Simeng Xiang, Zhanshan Wang, Zhe Zhang, and Zhong Zhang. "Effect of Annealing on Stress, Microstructure, and Interfaces of NiV/B4C Multilayers." Coatings 14, no. 4 (April 20, 2024): 513. http://dx.doi.org/10.3390/coatings14040513.

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The functionality and reliability of nanoscale multilayer devices and components are influenced by changes in stress and microstructure throughout fabrication, processing, and operation. NiV/B4C multilayers with a d-spacing of 3 nm were prepared by magnetron sputtering, and two groups of annealing experiments were performed. The stress, microstructure, and interface changes in NiV/B4C after annealing were investigated by grazing-incidence X-ray reflectometry (GIXR), grazing-incidence X-ray diffraction (GIXRD), X-ray diffuse scattering, and grazing-incidence small-angle X-ray scattering (GISAXS). The temperature dependence experiments revealed a gradual shift in the multilayer stress from compression to tension during annealing from 70 °C to 340 °C, with the stress approaching near-zero levels between 70 °C and 140 °C. The time-dependent experiments indicated that most of the stress changes occurred within the initial 10 min, which showed that prolonged annealing was unnecessary. Combining the X-ray diffraction and X-ray scattering measurements, it was found that the changes in the thickness, interface roughness, and lateral correlation length, primarily due to crystallization, drove the changes in stress and microstructure.

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Zhu, X., P. Predecki, M. Eatough, and R. Goebner. "Residual Stress Depth Profiling on Ground and on Polished Surfaces of an Al2O3/SiC(w) Composite." Advances in X-ray Analysis 39 (1995): 371–80. http://dx.doi.org/10.1154/s0376030800022783.

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This study uses the asymmetric grazing incidence x-ray diffraction (GIXD) method and related z-profile retrieval techniques to study the near surface residual stress depth proflles on ground and on polished surfaces of hot-pressed Al2O2SiC(w) composite specimen. The z-profiles of stress components σ11, σ22 and σ33 of the Al2O3 matrix were obtained by using the numerical inversion method as well as the inverse Laplace method. Both τ- and z-profiles of residual stresses are presented.

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Suturin, S. M., V. V. Fedorov, A. M. Korovin, G. A. Valkovskiy, S. G. Konnikov, M. Tabuchi, and N. S. Sokolov. "A look inside epitaxial cobalt-on-fluorite nanoparticles with three-dimensional reciprocal space mapping using GIXD, RHEED and GISAXS." Journal of Applied Crystallography 46, no. 4 (June 7, 2013): 874–81. http://dx.doi.org/10.1107/s0021889813008777.

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In this work epitaxial growth of cobalt on CaF2(111), (110) and (001) surfaces has been extensively studied. It has been shown by atomic force microscopy that at selected growth conditions stand-alone faceted Co nanoparticles are formed on a fluorite surface. Grazing-incidence X-ray diffraction (GIXD) and reflection high-energy electron diffraction (RHEED) studies have revealed that the particles crystallize in the face-centered cubic lattice structure otherwise non-achievable in bulk cobalt under normal conditions. The particles were found to inherit lattice orientation from the underlying CaF2 layer. Three-dimensional reciprocal space mapping carried out using X-ray and electron diffraction has revealed that there exist long bright 〈111〉 streaks passing through the cobalt Bragg reflections. These streaks are attributed to stacking faults formed in the crystal lattice of larger islands upon coalescence of independently nucleated smaller islands. Distinguished from the stacking fault streaks, crystal truncation rods perpendicular to the {111} and {001} particle facets have been observed. Finally, grazing-incidence small-angle X-ray scattering (GISAXS) has been applied to decouple the shape-related scattering from that induced by the crystal lattice defects. Particle faceting has been verified by modeling the GISAXS patterns. The work demonstrates the importance of three-dimensional reciprocal space mapping in the study of epitaxial nanoparticles.

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Ballard, B. L., P. K. Predecki, and D. N. Braski. "Stress-Depth Profiles in Magnetron Sputtered Mo Films Using Grazing Incidence X-Ray Diffraction (GIXD)." Advances in X-ray Analysis 37 (1993): 189–96. http://dx.doi.org/10.1154/s0376030800015688.

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AbstractIntrinsic stresses as a function of σ, the 1/e penetration depth were measured for a smooth, 1μm thick, fine grained, cylindrical post magnetron sputtered molybdenum film deposited on a vycor glass substrate in the dynamic deposition mode. Using grazing incidence diffraction and the Mo (321) reflection, lattice spacing profiles were determined for τ values from 200-4400 Å. The in-plane intrinsic stresses parallel and perpendicular to the post axis were determined employing the ϕ-integral method and assuming elastic isotropy. The results were related to the surface structure and composition profiles via atomic force microscopy (AFM) and auger electron spectroscopy (AES) respectively.

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Gidalevitz, D., R. Feidenhans'l, and L. Leiserowitz. "Determination of the crystal growth units by grazing incidence X-ray diffraction (GIXD) and AFM." Acta Crystallographica Section A Foundations of Crystallography 52, a1 (August 8, 1996): C514. http://dx.doi.org/10.1107/s0108767396079019.

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Predecki, Paul, X. Zhu, and B. Ballard. "Proposed Methods for Depth Profiling of Residual Stresses using Grazing Incidence X-Ray Diffraction (GIXD)." Advances in X-ray Analysis 36 (1992): 237–45. http://dx.doi.org/10.1154/s037603080001884x.

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AbstractTwo proposed methods are described for obtaining the depth profiles (τ-profiles) of strains and stresses as a function of the 1/e penetration depth τ, using GIXD in the asymmetric geometry, without the need for layer removal. In the first, the ψ-method: ψ is varied, for a given reflection, while holding τ constant, by varying the wavelength λ and adjusting the incident angle α so as to maintain τ constant. This allows dϕ,ψ vs Sin2ψ plots to be obtained at constant τ. In the second, the ϕ-integral method: interplanar spacings dϕ,ψ are measured for ϕ values from 0 to 2π, at constant ψ and τ by holding α fixed. Two ψ values, i.e. two wavelengths, are needed to obtain the whole strain tensor, but if the sample is quasi-isotropic and the stress state is biaxial, only one wavelength is needed. A direct method is also described for obtaining the profiles as a function of depth z (z-profiles) from the corresponding τ-profiles using inverse Laplace transforms. Application of the method to the residual strain vs τ data of Doerner and Brennan for an Al film on Si is presented.

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Cantelli, V., O. Geaymond, O. Ulrich, T. Zhou, N. Blanc, and G. Renaud. "TheIn situgrowth of Nanostructures on Surfaces (INS) endstation of the ESRF BM32 beamline: a combined UHV–CVD and MBE reactor forin situX-ray scattering investigations of growing nanoparticles and semiconductor nanowires." Journal of Synchrotron Radiation 22, no. 3 (April 9, 2015): 688–700. http://dx.doi.org/10.1107/s1600577515001605.

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This paper presents the upgraded `In situ growth of Nanoscructures on Surfaces' (INS) endstation of the InterFace beamline IF-BM32 at the European Synchrotron Radiation Facility (ESRF). This instrument, originally designed to investigate the structure of clean surfaces/interfaces/thin-films by surface X-ray diffraction, has been further developed to investigate the formation and evolution of nanostructures by combining small- and wide-angle X-ray scattering methodologies,i.e.grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction (GIXD). It consists of a UHV chamber mounted on az-axis type goniometer, equipped with residual gas analysis, reflection high-energy electron diffraction (RHEED) and Auger electron spectroscopy (AES) to complete the X-ray scattering investigations. The chamber has been developed so as up to eight sources of molecular beam epitaxy (MBE) can be simultaneously mounted to elaborate the nanostructures. A chemical vapor deposition (CVD) set-up has been added to expand the range of growing possibilities, in particular to investigatein situthe growth of semiconductor nanowires. This setup is presented in some detail, as well as the firstin situX-ray scattering measurements during the growth of silicon nanowires.

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Zhu, Xiaojing, and Paul Predecki. "Development of a Numerical Procedure for Determining the Depth Profiles of X-Ray Diffraction Data." Advances in X-ray Analysis 37 (1993): 197–203. http://dx.doi.org/10.1154/s037603080001569x.

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AbstractA numerical procedure is described and demonstrated for determining z-profiles from measured τ-profiles of diffraction data such as may be obtained by grazing incidence x-ray diffraction (GIXD). The z-profile was approximated by a piece wise linear function and the problem of solving the integral equation for the z-profile was thus converted to one of solving a set of linear equations. With a sufficient number of the linear pieces, the z-pTofile could be accurately determined. The procedure and its sensitivity to data errors was tested with several arbitrarily chosen known functions. It was found that when errors were introduced into either the τ-profile or the sample thickness D the resulting z-profiles become oscillatory.

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Hafidi, K., M. Azizan, Y. Ijdiyaou, and E. L. Ameziane. "Déposition par Pulvé Risation Cathodique Radio Fréquence et Caracté Risation Électronique, Structurale et Optique de Couches Minces du Dioxyde de Titane." Active and Passive Electronic Components 27, no. 3 (2004): 169–81. http://dx.doi.org/10.1080/08827510310001616885.

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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.

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Mukhopadhyay, Arun Kumar, Avishek Roy, Gourab Bhattacharjee, Sadhan Chandra Das, Abhijit Majumdar, Harm Wulff, and Rainer Hippler. "Surface Stoichiometry and Depth Profile of Tix-CuyNz Thin Films Deposited by Magnetron Sputtering." Materials 14, no. 12 (June 9, 2021): 3191. http://dx.doi.org/10.3390/ma14123191.

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We report the surface stoichiometry of Tix-CuyNz thin film as a function of film depth. Films are deposited by high power impulse (HiPIMS) and DC magnetron sputtering (DCMS). The composition of Ti, Cu, and N in the deposited film is investigated by X-ray photoelectron spectroscopy (XPS). At a larger depth, the relative composition of Cu and Ti in the film is increased compared to the surface. The amount of adventitious carbon which is present on the film surface strongly decreases with film depth. Deposited films also contain a significant amount of oxygen whose origin is not fully clear. Grazing incidence X-ray diffraction (GIXD) shows a Cu3N phase on the surface, while transmission electron microscopy (TEM) indicates a polycrystalline structure and the presence of a Ti3CuN phase.

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Hąc-Wydro, Katarzyna, Michał Flasiński, Marcin Broniatowski, Patrycja Dynarowicz-Łątka, and Jarosław Majewski. "Properties of β-sitostanol/DPPC monolayers studied with Grazing Incidence X-ray Diffraction (GIXD) and Brewster Angle Microscopy." Journal of Colloid and Interface Science 364, no. 1 (December 2011): 133–39. http://dx.doi.org/10.1016/j.jcis.2011.08.030.

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Nikolaev, K. V., I. A. Makhotkin, S. N. Yakunin, R. W. E. van de Kruijs, M. A. Chuev, and F. Bijkerk. "Specular reflection intensity modulated by grazing-incidence diffraction in a wide angular range." Acta Crystallographica Section A Foundations and Advances 74, no. 5 (September 1, 2018): 545–52. http://dx.doi.org/10.1107/s2053273318008963.

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Grazing-incidence X-ray diffraction (GID) is a well known technique for the characterization of crystal surfaces. A theoretical study has been performed of the sensitivity of GID to the structure of a crystal surface and distorted nanometre-thin surface layers. To simulate GID from crystals that have a complex subsurface structure, a matrix formalism of the dynamical diffraction theory has been applied. It has been found that the azimuthal rocking curves of a crystal that has a distorted subsurface, measured over a wide angular range, show asymmetric thickness oscillations with two distinguishable sets of frequencies: one corresponding to the diffraction in the single-crystal subsurface layer and the second corresponding to the diffraction in the single-crystal substrate. Therefore, azimuthal rocking curves allow characterization of the subsurface structure of a single crystal. Furthermore, thickness oscillations induced by evanescent diffraction modulate the specular reflection intensity, showing high-intensity modulations. This will potentially allow implementation of subsurface crystal characterization using, for instance, a laboratory-scale X-ray diffractometer.

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29

Nakayama, Yasuo, Masaki Iwashita, Mitsuru Kikuchi, Ryohei Tsuruta, Koki Yoshida, Yuki Gunjo, Yusuke Yabara, et al. "Electronic and Crystallographic Examinations of the Homoepitaxially Grown Rubrene Single Crystals." Materials 13, no. 8 (April 23, 2020): 1978. http://dx.doi.org/10.3390/ma13081978.

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Homoepitaxial growth of organic semiconductor single crystals is a promising methodology toward the establishment of doping technology for organic opto-electronic applications. In this study, both electronic and crystallographic properties of homoepitaxially grown single crystals of rubrene were accurately examined. Undistorted lattice structures of homoepitaxial rubrene were confirmed by high-resolution analyses of grazing-incidence X-ray diffraction (GIXD) using synchrotron radiation. Upon bulk doping of acceptor molecules into the homoepitaxial single crystals of rubrene, highly sensitive photoelectron yield spectroscopy (PYS) measurements unveiled a transition of the electronic states, from induction of hole states at the valence band maximum at an adequate doping ratio (10 ppm), to disturbance of the valence band itself for excessive ratios (≥ 1000 ppm), probably due to the lattice distortion.

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30

Landree, E., L. D. Marks, and P. Zschack. "Structure of the TiO2(100)-1X3 Surface Determined by Direct Methods." Microscopy and Microanalysis 3, S2 (August 1997): 1045–46. http://dx.doi.org/10.1017/s1431927600012113.

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An atomic model of the TiO2(100)-1x3 surface has been determined based on Grazing Incidence X-Ray Diffraction (GIXD) data analyzed by direct methods coupled with χ2 minimization. The final model has every surface octahedral site occupied, and resembles the NaCl structure, in contrast to the normal structure of bulk rutile which has half of the sites occupied (Fig. 1). This structure is non-stoichiometric which is consistent with the observed spectroscopic data that indicates that the surface is titanium rich. The structure contains edge and face sharing octahedra, present in other known defect structures in TiO2, and appear consistent with what has been observed in Scanning Tunneling Microscopy.The data consisted of 19 measured structure factors acquired from GIXD. The phases for the measured beams were calculated using a Sayre equation with Unitary Structure factors and a Genetic Algorithm global search technique. Based upon the calculated phases, charge density maps were constructed and used to determine the positions of titanium atoms within the unit cell (Fig. 2).

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CUI, S. F., Z. H. MAI, C. Y. WANG, L. S. WU, J. T. OUYANG, and J. H. LI. "X-RAY ANALYSIS OF Si1−xGex/Si SUPERLATTICES." Modern Physics Letters B 05, no. 23 (October 10, 1991): 1591–97. http://dx.doi.org/10.1142/s0217984991001891.

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We present the studies on the correlation between the structural parameters of the well and the barrier in Si 1−x Ge x/ Si quantum well superlattices by using X-ray grazing incidence diffraction (GID) under total external reflection conditions and the conventional X-ray double-crystal diffraction. Both the coherent growth and the partial relaxed growth in the interfaces between the two components of the superlattices were found by the GID technique. The GID technique gave the valuable information that the relaxation occurs in the interfaces between the two components of the superlattices which cannot be distinguished by other analytical tools. This shows the potential of the depth-controlled analysis for superlattices by the GID technique.

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32

Ravanbakhsh, Arsalan, Fereshteh Rashchi, M. Heydarzadeh Sohi, and Rasoul Khayyam Nekouei. "Synthesis of Nanostructured Zinc Oxide Thin Films by Anodic Oxidation Method." Advanced Materials Research 829 (November 2013): 347–51. http://dx.doi.org/10.4028/www.scientific.net/amr.829.347.

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In this study, the ZnO thin film was synthesized by means of anodic oxidation method. A basic solution containing NaOH and NH4Cl as additive was used for the process. Effect of time and voltage on the microstructure of the obtained thin film has been studied. Characterization has been performed using grazing incidence X-ray diffraction (GIXD), field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). Nanostructured thin film has been obtained with different morphologies according to different process parameters. FESEM analysis indicated that as the process time increases, the morphology of the film changes from grooved surface into flaky porous structure. It was also evident that hexagonal shaped simonkolleite formed during the process which was then transformed into zinc oxide and zinc chloride by heat treating.

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33

Yunin P. A., Nazarov A. A., and Potanina E. A. "Application of the GIXRD Technique to Investigation of Damaged Layers in NaNd(WO_4)-=SUB=-2-=/SUB=- and NaNd(MoO_4)-=SUB=-2-=/SUB=- Ceramics Irradiated with High-Energy Ions." Technical Physics 92, no. 8 (2022): 956. http://dx.doi.org/10.21883/tp.2022.08.54556.69-22.

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The technique of grazing incidence X-ray diffractometry (GIXRD) was used to study damaged layers in NaNd(WO_4)2 and NaNd(MoO_4)2 ceramics irradiated with high-energy ions. The possibilities and applicability limits of the technique for the analysis of such samples are shown. Estimates of the degree of amorphization in near-surface layers of ceramics are given depending on the irradiation dose. The higher resistance of NaNd(MoO_4)2 ceramics to external radiation exposure as compared to NaNd(WO_4)2 has been demonstrated. Keywords: X-ray diffraction, Parallel beam method, Grazing incidence geometry, Ion irradiation, Ceramics, Radiation resistance, Amorphization, Damaged layer.

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34

Gunjo, Yuki, Hajime Kamebuchi, Ryohei Tsuruta, Masaki Iwashita, Kana Takahashi, Riku Takeuchi, Kaname Kanai, et al. "Interface Structures and Electronic States of Epitaxial Tetraazanaphthacene on Single-Crystal Pentacene." Materials 14, no. 5 (February 26, 2021): 1088. http://dx.doi.org/10.3390/ma14051088.

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The structural and electronic properties of interfaces composed of donor and acceptor molecules play important roles in the development of organic opto-electronic devices. Epitaxial growth of organic semiconductor molecules offers a possibility to control the interfacial structures and to explore precise properties at the intermolecular contacts. 5,6,11,12-tetraazanaphthacene (TANC) is an acceptor molecule with a molecular structure similar to that of pentacene, a representative donor material, and thus, good compatibility with pentacene is expected. In this study, the physicochemical properties of the molecular interface between TANC and pentacene single crystal (PnSC) substrates were analyzed by atomic force microscopy, grazing-incidence X-ray diffraction (GIXD), and photoelectron spectroscopy. GIXD revealed that TANC molecules assemble into epitaxial overlayers of the (010) oriented crystallites by aligning an axis where the side edges of the molecules face each other along the [1¯10] direction of the PnSC. No apparent interface dipole was found, and the energy level offset between the highest occupied molecular orbitals of TANC and the PnSC was determined to be 1.75 eV, which led to a charge transfer gap width of 0.7 eV at the interface.

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35

Magdans, Uta, Hermann Gies, Xavier Torrelles, and Jordi Rius. "Investigation of the {104} surface of calcite under dry and humid atmospheric conditions with grazing incidence X-ray diffraction (GIXRD)." European Journal of Mineralogy 18, no. 1 (March 6, 2006): 83–92. http://dx.doi.org/10.1127/0935-1221/2006/0018-0083.

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36

Stabenow, Rainer, and Alfried Haase. "New Tools for Grazing Incidence Diffraction Measurements: Comparison of Different Primary and Secondary Beam Conditioners." Advances in X-ray Analysis 39 (1995): 87–94. http://dx.doi.org/10.1154/s0376030800022485.

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Grazing incidence diffraction (GID) is a powerful tool for the structural characterization of thin films. Unlike traditional Bragg-Brentano geometry (divergent X-ray beam, focusing geometry), GID experiments are enhanced by a parallel beam of high intensity. Classical conditioning of the X-ray beam is done by using small slits on the primary beam side and a long Soller slit in combination with a flat crystal (e.g. graphite, lithium fluoride or germanium) or an energy dispersive detector on the secondary beam side. However, new alternatives for beam conditioners are becoming available which promise increased performance. X-ray beam optics using either planar or graded parabolically curved multilayer mirrors of high reflectivity have been constructed for the primary beam side as well as for the secondary beam side.

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37

Wang, Po-Wen. "Structural Characterization of Magnetic Recording Media by Using Grazing Incident and Conventional X-Ray Diffraction." Advances in X-ray Analysis 36 (1992): 197–202. http://dx.doi.org/10.1154/s0376030800018796.

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In recent years, the microstructure of Co-based alloy magnetic thin film disks has been studied extensively by using a conventional x-ray diffraction (XRD) technique(1-4). Efforts to understand the relationship between the microstructure and the magnetic properties of disk had been limited due to the lack of depth resolution in the conventional theta-2theta scanning technique. In this paper, a fixed 0.5 degree of grazing incidence(5) 2-theta scan X-ray diffraction (GIXRD) technique was used to characterize the thin film disk microstructure and therefore to correlate with the magnetic properties.

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38

Ballard, B. L., X. Zhu, P. K. Predecki, D. Albin, A. Gabor, J. Turtle, and R. Noufi. "Determination of Composition and Phase Depth-Profiles in Multilayer and Gradient Solid Solution Photovoltaic Films Using Grazing Incidence X-ray Diffraction." Advances in X-ray Analysis 38 (1994): 269–76. http://dx.doi.org/10.1154/s0376030800017882.

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Abstract A method for using grazing incidence x-ray diffraction (GIXD) for profiling composition changes with depth of photovoltaic quality thin films is presented. The average thickness of the first layer in a multi-layer film of CuIn2Se3.5/CuInSe2/Mo and the variation in solid solution composition of a Cu(In1-xGax)Se2 (CIGS) film with depth are solved using this method. The phase volume fraction and the phase composition profiles are developed from peak intensity and d-spacing measurements respectively at a series of fixed incident angles corresponding to a set of increasing 1/e penetration depths, τ. Inverse Laplace and numerical methods are applied to the τ profiles converting them to true depth profiles. Vegard's law is applied to the d-spacing vs z-profile to obtain x in the formula Cu(In1-xGax)Se2. The results show that an ∼1 μm thick layer of CuIn2Se3.5 is present on the surface of the multi-layer film and that the CIGS film consists of a Ga rich surface layer ∼2000 Å thick followed by a gradual decrease in Ga content with increasing depth. This gradient appears to be desirable for producing photovoltaic quality CIGS films.

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39

Takayama, Shinji. "Measurement of Internal Stresses Exerted in an Each Layer of Multiple Layer's Film with Temperature Using a Grazing Incidence X-Ray Diffraction." ECS Meeting Abstracts MA2022-01, no. 23 (July 7, 2022): 1131. http://dx.doi.org/10.1149/ma2022-01231131mtgabs.

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The internal stresses in an each layer of multiple layer's film (AZO, Cu, and Mo) has been measured experimentally using grazing incidence X-ray diffraction. This was performed utilizing the difference of total reflection values between consisting layers so as to be able to measure the each internal stresses in turn by the GISD.

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40

Aliouat, Mouaad Yassine, Dmitriy Ksenzov, Stephanie Escoubas, Jörg Ackermann, Dominique Thiaudière, Cristian Mocuta, Mohamed Cherif Benoudia, David Duche, Olivier Thomas, and Souren Grigorian. "Direct Observations of the Structural Properties of Semiconducting Polymer: Fullerene Blends under Tensile Stretching." Materials 13, no. 14 (July 10, 2020): 3092. http://dx.doi.org/10.3390/ma13143092.

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We describe the impact of tensile strains on the structural properties of thin films composed of PffBT4T-2OD π-conjugated polymer and PC71BM fullerenes coated on a stretchable substrate, based on a novel approach using in situ studies of flexible organic thin films. In situ grazing incidence X-ray diffraction (GIXD) measurements were carried out to probe the ordering of polymers and to measure the strain of the polymer chains under uniaxial tensile tests. A maximum 10% tensile stretching was applied (i.e., beyond the relaxation threshold). Interestingly we found different behaviors upon stretching the polymer: fullerene blends with the modified polymer; fullerene blends with the 1,8-Diiodooctane (DIO) additive. Overall, the strain in the system was almost twice as low in the presence of additive. The inclusion of additive was found to help in stabilizing the system and, in particular, the π–π packing of the donor polymer chains.

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41

Ballard, B. L., P. K. Predecki, T. R. Watkins, K. J. Kozaczek, D. N. Braski, and C. R. Hubbard. "Depth Profiling Biaxial Stresses in Sputter Deposited Molybdenum Films; Use of the Cos2φ Method." Advances in X-ray Analysis 39 (1995): 363–70. http://dx.doi.org/10.1154/s0376030800022771.

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Depth profiles of intrinsic in-plane, biaxial stresses were obtained as a function of τ, the 1/e penetration depth, in a 1.0 um thick planar d. c. magentron sputter deposited molybdenum film using asymmetric grazing incidence x-ray diffraction (GIXD). τ was varied between 20 and 276 Å. The stresses σ11 and σ22 were characterized in the directions parallel and perpendicular to the long axis of the cathode respectively using a cos2φ method. The results show that starting from τ=17Å, σ11 and σ22 are compressive and become rapidly more compressive with a minimum at τ ∼ 20 - 40 Å thereafter increasing gradually toward tensile values. The reasons for the shape of the stress gradient are not well understood but may be related to the relaxation of the stresses at the tops of the columnar Zone T-type microstructure and to the oxygen gradient in the film.

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Eatough, Michael O., and Raymond P. Gochner. "The Effects of Using Long Soller Slits as “Parallel Beam Optics” for Gixrd on Diffraction Data." Advances in X-ray Analysis 37 (1993): 167–73. http://dx.doi.org/10.1154/s0376030800015652.

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AbstractGrazing incidence x-ray diffraction (GIXRD) using long soller slit assemblies and a flat crystal monochromator, sometimes referred to as thin film optics, are used to study poly crystal line thin films, polymers, metals, etc. The unique ability of GIXRD to characterize crystalline materials as function of depth and provide accurate strain measurements has lead to the growing popularity of this technique. This non-focusing pseudo-parallel beam geometry can produce various effects on diffraction data which can make interpretation difficult Artifacts such as peak splitting, kα2 distortion, and peaks which shift dramatically as a function of grazing incidence angle are observed when using GIXRD. These artifacts can be related to grazing incidence angle, the divergence of the soller plates, the thickness of the soller plates, the substrate material, and the type of monochromator used. This paper briefly describes some of the topics discussed at the 1992 & 1993 Denver Conferences workshops on parallel beam optics.

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43

Achilli, Elisabetta, Filippo Annoni, Nicola Armani, Maddalena Patrini, Marina Cornelli, Leonardo Celada, Melanie Micali, Antonio Terrasi, Paolo Ghigna, and Gianluca Timò. "Capabilities of Grazing Incidence X-ray Diffraction in the Investigation of Amorphous Mixed Oxides with Variable Composition." Materials 15, no. 6 (March 15, 2022): 2144. http://dx.doi.org/10.3390/ma15062144.

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X-ray Diffraction has been fully exploited as a probe to investigate crystalline materials. However, very little research has been carried out to unveil its potentialities towards amorphous materials. In this work, we demonstrated the capabilities of Grazing Incidence X-ray Diffraction (GIXRD) as a simple and fast tool to obtain quantitative information about the composition of amorphous mixed oxides. In particular, we evidenced that low angle scattering features, associated with local structure parameters, show a significant trend as a function of the oxide composition. This evolution can be quantified by interpolating GIXRD data with a linear combination of basic analytical functions, making it possible to build up GIXRD peak-sample composition calibration curves. As a case study, the present method was demonstrated on Ta2O5–SiO2 amorphous films deposited by RF-magnetron sputtering. GIXRD results were validated by independent measurement of the oxide composition using Rutherford Backscattering Spectrometry (RBS). These materials are attracting interest in different industrial sectors and, in particular, in photovoltaics as anti-reflection coatings. Eventually, the optical properties measured by spectroscopic ellipsometry were correlated to the chemical composition of the film. The obtained results highlighted not only a correlation between diffraction features and the composition of amorphous films but also revealed a simple and fast strategy to characterize amorphous thin oxides of industrial interest.

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Suturin, S. M., V. V. Fedorov, A. M. Korovin, N. S. Sokolov, A. V. Nashchekin, and M. Tabuchi. "Epitaxial Ni nanoparticles on CaF2(001), (110) and (111) surfaces studied by three-dimensional RHEED, GIXD and GISAXS reciprocal-space mapping techniques." Journal of Applied Crystallography 50, no. 3 (May 16, 2017): 830–39. http://dx.doi.org/10.1107/s160057671700512x.

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The development of growth techniques aimed at the fabrication of nanoscale heterostructures with layers of ferroic 3dmetals on semiconductor substrates is very important for their potential usage in magnetic media recording applications. A structural study is presented of single-crystal nickel island ensembles grown epitaxially on top of CaF2/Si insulator-on-semiconductor heteroepitaxial substrates with (111), (110) and (001) fluorite surface orientations. The CaF2buffer layer in the studied multilayer system prevents the formation of nickel silicide, guides the nucleation of nickel islands and serves as an insulating layer in a potential tunneling spin injection device. The present study, employing both direct-space and reciprocal-space techniques, is a continuation of earlier research on ferromagnetic 3dtransition metals grown epitaxially on non-magnetic and magnetically ordered fluorides. It is demonstrated that arrays of stand-alone faceted nickel islands with a face-centered cubic lattice can be grown controllably on CaF2surfaces of (111), (110) and (001) orientations. The proposed two-stage nickel growth technique employs deposition of a thin seeding layer at low temperature followed by formation of the islands at high temperature. The application of an advanced three-dimensional mapping technique exploiting reflection high-energy electron diffraction (RHEED) has proved that the nickel islands tend to inherit the lattice orientation of the underlying fluorite layer, though they exhibit a certain amount of {111} twinning. As shown by scanning electron microscopy, grazing-incidence X-ray diffraction (GIXD) and grazing-incidence small-angle X-ray scattering (GISAXS), the islands are of similar shape, being faceted with {111} and {100} planes. The results obtained are compared with those from earlier studies of Co/CaF2epitaxial nanoparticles, with special attention paid to the peculiarities related to the differences in lattice structure of the deposited metals: the dual-phase hexagonal close-packed/face-centered cubic lattice structure of cobalt as opposed to the single-phase face-centered cubic lattice structure of nickel.

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Huang, Wenjie, Meng Sun, Wen Wen, Junfeng Yang, Zhuoming Xie, Rui Liu, Xianping Wang, Xuebang Wu, Qianfeng Fang, and Changsong Liu. "Strain Profile in the Subsurface of He-Ion-Irradiated Tungsten Accessed by S-GIXRD." Crystals 12, no. 5 (May 12, 2022): 691. http://dx.doi.org/10.3390/cryst12050691.

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The strain profile in the subsurface of He-ion-irradiated W was figured out by unfolding the synchrotron-grazing incidence X-ray diffraction (S-GIXRD) patterns at different incidence angles. The results show that for 2 × 1021 ions/m2 He2+-irradiated W, in addition to a compressive strain exists in the depths of 0–100 nm due to mechanical polishing, an expansion strain appears in the depth beyond 100 nm owing to irradiation-induced lattice swelling. This work provides a reference for the study of irradiation damage in the subsurface by S-GIXRD.

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Veder, Jean-Pierre, Ayman Nafady, Graeme Clarke, Roland De Marco, and Alan M. Bond. "A Combined Voltammetric and Synchrotron Radiation-Grazing Incidence X-ray Diffraction Study of the Electrocrystallization of Zinc Tetracyanoquinodimethane." Australian Journal of Chemistry 65, no. 3 (2012): 236. http://dx.doi.org/10.1071/ch11361.

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The in situ electrocrystallization of zinc tetracyanoquinodimethane (TCNQ) has been explored using synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD) at potentials in the region of the cyclic voltammetric peak where reduction of TCNQ to TCNQ– occurs at a Pt electrode in acetonitrile (0.1 M [NBu4][PF6]) solution containing Zn(NO3)2·6H2O. The in situ SR-GIXRD data along with ex situ IR and Raman spectroscopy results all confirmed the formation of the kinetically favoured phase of Zn[TCNQ]2(H2O)2 as the product.

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47

Wroński, S., K. Wierzbanowski, A. Baczmański, A. Lodini, Ch Braham, and W. Seiler. "X-ray grazing incidence technique—corrections in residual stress measurement—a review." Powder Diffraction 24, S1 (June 2009): S11—S15. http://dx.doi.org/10.1154/1.3139054.

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Using X-ray grazing incidence diffraction (GID) it is possible to perform a nondestructive analysis of the heterogeneous stress field for different volumes below the surface of the sample. 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 easily changed by an appropriate selection of α angle (or also by using a different type of radiation). There are, however, some factors which have to be corrected in this technique. The most important is the refraction of X-ray wave: it changes the wavelength and direction of the beam. Both effects modify a pick position. A corresponding correction was calculated and tested on ferrite powder and on 316L austenite stainless steel sample.

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Grossner, Ulrike, Marco Servidori, Marc Avice, Ola Nilsen, Helmer Fjellvåg, Roberta Nipoti, and Bengt Gunnar Svensson. "X-Ray and AFM Analysis of Al₂O₃ Deposited by ALCVD on n-Type 4H-SiC." Materials Science Forum 556-557 (September 2007): 683–86. http://dx.doi.org/10.4028/www.scientific.net/msf.556-557.683.

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Al2O3 grown by Atomic Layer Chemical Vapour Deposition (ALCVD) on n-type 4H-SiC with a nominal thickness of 100nm has been characterized by Grazing Incidence X-Ray Diffraction (GIXD) and Specular X-Ray Reflectivity (SXR) measurements. After post-deposition, the samples were annealed at different temperatures and durations in argon atmosphere. The GIXD results reveal crystallization at temperatures above 900°C, most likely in the form of θ-Al2O3 or γ-Al2O3. However, the formation of a new, non-stoichiometric Al2O3 phase cannot be excluded. The crystalline domain size, evaluated from the peak FWHMs after subtraction of the instrumental broadening, is found to be almost equal (18±1nm), independent of T in the range 900°C≤T≤1100°C and time in the range 1h≤t≤3h. From SXR, mass density profiles are derived. Whereas the as grown film exhibits the lowest mass density, at 800°C a low-density interface layer forms. At the same time, it appears that the initial crystallization starts at the surface. At 900°C, the density increases sharply (this process involves film crystallization) and the film thickness correspondingly reduces. Whereas the density increase and thickness reduction still continue for T>900°C (tendency to the density α-Al2O3), the density of the interfacial layer has a minimum at 900°C and gradually increases for higher temperatures. From Atomic Force Microscopy (AFM) investigations it could be revealed that the starting of the crystallization at 900°C is accompanied with a substantial surface roughening. For annealing at higher temperatures, the surface roughness is in the range of the one of the as-grown sample (about 6Å).

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Novák, Patrik, Aleksandr Gokhman, Edmund Dobročka, Jozef Bokor, and Stanislav Pecko. "Investigation Of Helium Implanted Fe–Cr Alloys By Means Of X–Ray Diffraction And Positron Annihilation Spectroscopy." Journal of Electrical Engineering 66, no. 6 (November 1, 2015): 334–38. http://dx.doi.org/10.2478/jee-2015-0055.

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Abstract X-ray diffraction (XRD) and positron annihilation spectroscopy (PAS) have been used for the characterization of the two binary alloys Fe-Cr with Cr content 2.36 and 8.39 wt%. The influence of ion implantation on these alloys was studied. Different implantation doses of helium, up to 0.5 C/cm2, were used to simulate neutron-induced damage in a sub-surface region. To characterize the damage, a lattice parameter, coherent domain size, residual stress and a crystallographic texture have been studied by grazing incidence X-ray diffraction (GIXRD). It was found out that these parameters showed a similar dependence on the implantation dose as the positron lifetime determined by positron annihilation spectroscopy.

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Yi, Jian, Xiao Dong He, Yue Sun, Zhi Peng Xie, Wei Jiang Xue, and Fen Yan Cao. "GIAXD and XPS Characterization of sp³C Doped SiC Superhard Nanocomposite Film." Key Engineering Materials 512-515 (June 2012): 971–74. http://dx.doi.org/10.4028/www.scientific.net/kem.512-515.971.

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The sp3C doped SiC superhard nanocomposite films had been deposited on stainless steel (SS) substrates at different temperature by electron beam-physical vapor deposition (EB-PVD). The sp3C doped SiC film was studied by grazing incidence X-ray asymmetry diffraction (GIAXD), and X-ray photoelectron spectroscopy (XPS). The results of GIAXD showed that the sp3 doped SiC nanocomposite films were not perfect crystalline, which was composed with fine SiC nanocrystals, and a second phase very similar with diamond like carbon (DLC). XPS analysis showed that the excess C existing in films and turned from diamond into DLC from the surface to inner of film.

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Journal articles on the topic 'Grazing incidence X-ray diffraction (GIXD)'

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