Ab initio determination of the framework structure of the heavy-metal oxide CsxNb2.54W2.46O14 from 100kV precession electron diffraction data

Weirich, Thomas E.; Portillo, J.; Cox, Gerhard; Hibst, H.; Nicolopoulos, Stavros

doi:10.1016/j.ultramic.2005.07.002

Cited by 80 publications

(63 citation statements)

References 35 publications

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“…Alternative methods for relaxation of thickness restriction use high voltage electron microscopy (HVEM) and a newly developed electron diffraction method, precession electron diffraction (PED) method. 26,27 In the study of electron diffraction data by HVEM, dynamical scattering effects are expected to be reduced because of its longer mean free path and extended Ewald sphere by higher transmission power. Application of the PED method is also expected to reduce the dynamical scattering considerably by employing conical beam illumination and rapid precession.…”

Section: Discussionmentioning

confidence: 99%

Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction

Kim

Seo

Cheon³

et al. 2009

Bulletin of the Korean Chemical Society

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The structure of nano-crystalline MnFe2O4 was determined and refined with electron powder diffraction data employing the Rietveld refinement technique. A nano-crystalline sample (with average crystal size of about 10.9 nm) was characterized by selected area electron diffraction in an energy-filtering transmission electron microscope operated at 120 kV. All reflection intensities were extracted from a digitized image plate using the program ELD and then used in the course of structure refinements employing the program FULLPROF for the Rietveld analysis. The final structure was refined in space group Fd-3m (# 227) with lattice parameters a=8.3413(7) Å. The reliability factors of the refinement are RF=7.98% and RB=3.55%. Comparison of crystallographic data between electron powder diffraction data and reference data resulted in better agreement with ICSD-56121 rather than with ICSD-28517 which assumes an initial structure model.Key Words: Nano-crystalline MnFe 2 O 4 , Rietveld analysis, Electron powder diffraction, Energy filtering, Image plate Figure 1. Bright-field image of MnFe2O4 nano-crytalline and the corresponding selected area electron powder diffraction. The overlay on the electron diffraction shows the average intensity profile that was used to determine the structure.

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Section: Discussionmentioning

confidence: 99%

Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction

Kim

Seo

Cheon³

et al. 2009

Bulletin of the Korean Chemical Society

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“…Despite such low-dose settings relatively short exposure times up to 1s need to be selected in the case of high-resolution images. Another breakthrough for the investigation of air sensitive samples is given by the precession electron diffraction technique (PED) [11][12][13][14][15]. The PED technique with the electron beam moving on a precession cone (precession angle of 3°) minimizes multiple scattering and beyond that is superior to selected area electron diffraction (SAED, fixed beam), since the PED experiments overcome the time consuming adjustment of the precise zone axis orientation of the sample.…”

Section: Experimental and Methodsmentioning

confidence: 99%

Electron Microscopy Investigations on Highly Beam and Moisture Sensitive Samples – the System Li/Ba/Ca

Kienle¹,

Smetana²,

Düppel³

et al. 2010

Zeitschrift anorg allge chemie

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“…2). Although the PED intensities are still not ideal, they are significantly improved over typical SAED intensities [24], and have been used to solve several structures [25][26][27][28][29].…”

Section: Precession Electron Diffraction (Ped)mentioning

confidence: 99%

“…Precession electron diffraction data have already been used in combination with direct methods and maximum entropy methods to determine two-dimensional structures [25][26][27][28]. This is an indication that the reflection intensities are reliable enough and have sufficient resolution for the phasing process to succeed.…”

Section: Phase Retrieval From Ped Data Using Charge Flippingmentioning

confidence: 99%

Electron crystallography as a complement to X-ray powder diffraction techniques

McCusker¹,

Baerlocher²

2013

Zeitschrift für Kristallographie - Crystalline Materials

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Abstract. Electron microscopy techniques yield information for crystal structure analysis that is remarkably complementary to that obtained from X-ray powder diffraction data. Structures of polycrystalline materials that resist solution by either method alone can sometimes be solved by combining the two. For example, the intensities extracted from an X-ray powder diffraction pattern are kinematical and can be interpreted easily, while those obtained from a typical selected area electron diffraction (SAED) or precession electron diffraction (PED) pattern are at least partially dynamical and therefore more difficult to use directly. On the other hand, many reflections in a powder diffraction pattern overlap and only the sum of their intensities can be measured, while those in an electron diffraction pattern are from a single crystal and therefore well separated in space. Although the intensities obtained from either SAED or PED data are less reliable than those obtained with Xrays, they can be used to advantage to improve the initial partitioning of the intensities of overlapping reflections. However, it is the partial crystallographic phase information that can be extracted either from high-resolution transmission electron microscopy (HRTEM) images or from PED data that has proven to be particularly useful in combination with high-resolution X-ray powder diffraction data. The dual-space (reciprocal and real space) structure determination programs Focus and Superflip have been shown to be especially useful for combining the two different types of data.

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Ab initio determination of the framework structure of the heavy-metal oxide CsxNb2.54W2.46O14 from 100kV precession electron diffraction data

Cited by 80 publications

References 35 publications

Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction

Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction

Electron Microscopy Investigations on Highly Beam and Moisture Sensitive Samples – the System Li/Ba/Ca

Electron crystallography as a complement to X-ray powder diffraction techniques

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Ab initio determination of the framework structure of the heavy-metal oxide CsxNb2.54W2.46O14 from 100kV precession electron diffraction data

Cited by 80 publications

References 35 publications

Rietveld Analysis of Nano-crystalline MnFe2O4with Electron Powder Diffraction

Rietveld Analysis of Nano-crystalline MnFe2O4with Electron Powder Diffraction

Electron Microscopy Investigations on Highly Beam and Moisture Sensitive Samples – the System Li/Ba/Ca

Electron crystallography as a complement to X-ray powder diffraction techniques

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Product

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Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction

Rietveld Analysis of Nano-crystalline MnFe₂O₄with Electron Powder Diffraction