A method for the accurate determination of crystal truncation rod intensities by X-ray diffraction

Specht, E. D.; Walker, Frederick J.

doi:10.1107/s0021889892011592

Cited by 35 publications

(41 citation statements)

References 4 publications

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“…This is largely due to the use of point (or linear) detectors. For the large acceptance required in the stationary mode a large amount of background is then collected and it is necessary to measure the background by rotating the crystal over a sufficiently wide angle (Specht & Walker, 1993). These extra 'scans' significantly lower the ratio in (64).…”

Section: Discussionmentioning

confidence: 99%

Integrated Intensities Using a Six-Circle Surface X-ray Diffractometer

Vlieg¹

1997

J Appl Crystallogr

298

267

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The geometrical and resolution corrections are derived that occur in the measurement of the integrated intensities of surface diffraction rods for the case of a sixcircle diffractometer. Since the six-circle geometry entails as special cases the five-circle and the z-axis diffractometers, the results are valid for these geometries as well. The derivations are valid for any incoming or outgoing angle of the X-ray beam, and are particularly important for measurements at large perpendicular momentum transfer. Expressions are derived for the integrated intensity from rocking scans, from stationary measurements and from reflectivity data. With all correction factors known, it is possible to derive the structure factors with a common scale factor from all these types of scans. It is expected that area detectors combined with stationary measurements will find widespread use in the surface X-ray diffraction community.

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Section: Discussionmentioning

confidence: 99%

Integrated Intensities Using a Six-Circle Surface X-ray Diffractometer

Vlieg¹

1997

J Appl Crystallogr

298

267

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“…We compile the full pole figure by appropriately merging the [intensity, χ] data sets extracted from the local-specular diffraction pattern and the grazing incidence diffraction pattern. To determine an appropriate merging angle for these two data sets, we plot intensity vs. A Lorentz correction [36][37][38] is required in X-ray geometries that involves either a rotating single crystal or a stationary powder sample. However, in the present case of morphology quantification (as opposed to structural characterization) the data are obtained from a single Bragg ring, which obviates the need for a Lorentz correction.…”

Section: χ-Correctionmentioning

confidence: 99%

Quantification of Thin Film Crystallographic Orientation Using X-ray Diffraction with an Area Detector

Baker¹,

et al. 2010

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As thin films become increasingly popular (for solar cells, LEDs, microelectronics, batteries), quantitative morphological and crystallographic information is needed to predict and optimize the film's electronic, optical and mechanical properties. This quantification can be obtained quickly and easily with X-ray diffraction using an area detector in two simple sample geometries. In this paper, we describe a methodology for constructing complete pole figures for thin films with fiber texture (isotropic in-plane orientation). We demonstrate this technique on semicrystalline polymer films, self-assembled nanoparticle semiconductor films, and randomlypacked metallic nanoparticle films. This method can be immediately implemented to help 2 understand the relationship between film processing and microstructure, enabling the development of better and less expensive electronic and optoelectronic devices.Keywords: grazing-incidence X-ray diffraction; pole figure; texture analysis; morphology; thin film IntroductionThe optical and electronic properties of polycrystalline and semicrystalline materials are highly dependent on the materials' morphology. When these properties are anisotropic in the single crystal form, the corresponding bulk properties of the poly-or semi-crystalline material are often dependent upon the orientation distribution of the crystallites.1 As efforts are made to optimize the electrical and optical properties of functional, solution-processed polycrystalline films used for thin film transistors, solar cells, and other emerging technologies, it is necessary to fully characterize the orientation distribution, or texture, of the crystallites. There has been much effort devoted to correlating the microstructure and properties of thin films (<100 nm) of nanostructured organic semiconductors 2-7 and inorganic semiconducting nanoparticles 8,9 , but the collection of complete texture information is often challenging due to the limited film thickness.In this work, we introduce an X-ray diffraction-based method for collecting and constructing quantitative pole figures with an area detector for thin films with isotropic crystallographic orientation in the substrate plane (classically referred to as fiber texture). The technique is rapid and ideal for thin films that are sensitive to beam damage, diffract weakly or are otherwise limited by their thin film form to certain diffraction geometries. 3A pole figure is a plot of the orientation distribution of a particular set of crystallographic lattice planes, providing a useful illustration of a material's texture. Traditional pole figures of bulk samples can be collected in either reflection or transmission mode. Pole figures collected in a reflection mode utilize a symmetric geometry introduced by Schultz 10-12 . In this technique, diffraction intensities are collected using a point detector as the sample is rotated along two axes.Accurate collection of intensity in the Schultz geometry is generally limited to within 85° of the surface normal, due to distortions t...

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“…The instrument function depends on the wavelengths passed by the monochromator, the divergence of the beam and the angular acceptance of the detector (Munkholm et al, 1997). In our experimental set-up, the shape of the instrument function is mainly dominated by the large angular acceptance of the detector: 8 mrad in the scattering plane and 2 mrad perpendicular to the scattering plane, which is a consequence of using the slit setting of Specht & Walker (1993). The angular acceptance results in a plane of allowed scattering vectors that is inclined with respect to the rod.…”

Section: Resultsmentioning

confidence: 99%

“…The total width 3 of the CTR as measured using a rocking curve is a function of the horizontal angular acceptance of detector b and can be derived from equation (10) given by Specht & Walker (1993) as w ba2tan 1acos X 23…”

Section: Resultsmentioning

confidence: 99%

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Influence of miscut on crystal truncation rod scattering

Munkholm¹,

Brennan²

1999

J Appl Cryst

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X-rays can be used to measure the roughness of a surface by the study of crystal truncation rod scattering. It is shown that for a simple cubic lattice the presence of a miscut surface with a regular step array has no effect on the scattered intensity of a single rod and that a distribution of terrace widths on the surface is shown to have the same effect as adding roughness to the surface. For a perfect crystal without miscut, the scattered intensity is the sum of the intensity from all the rods with the same in-plane momentum transfer. For all real crystals, the scattered intensity is better described as that from a single rod. It is shown that data-collection strategies must correctly account for the sample miscut or there is a potential for improperly measuring the rod intensity. This can result in an asymmetry in the rod intensity above and below the Bragg peak, which can be misinterpreted as being due to a relaxation of the surface. The calculations presented here are compared with data for silicon (001) wafers with 0.1 and 4 miscuts.

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A method for the accurate determination of crystal truncation rod intensities by X-ray diffraction

Cited by 35 publications

References 4 publications

Integrated Intensities Using a Six-Circle Surface X-ray Diffractometer

Integrated Intensities Using a Six-Circle Surface X-ray Diffractometer

Quantification of Thin Film Crystallographic Orientation Using X-ray Diffraction with an Area Detector

Influence of miscut on crystal truncation rod scattering

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