Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials

Mugnaioli, Enrico; Kolb, Ute

doi:10.1016/j.micromeso.2012.02.024

Cited by 37 publications

(37 citation statements)

References 42 publications

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“…71 The Zn and N atoms could be positioned using RED data, whereas C atoms were additionally inserted according to geometry of the imidazole ligand. ADT was employed for structure solutions of Cu-benzene-1-3-5-tricarboxylate (HKUST-1), 72 Zn-BTDD (MFU-4, BTDD = bis(1H-1,2,3-triazolo- [4,5-b], [4,5- 58 Bi-benzenetrisbenzoate (CAU-7) 73 and Zr-terephthalate (UiO-66) 74 . These methodologies can only be applied for structure determination of very limited assortment of highly stable MOF systems with the strong support of complementary methods.…”

Section: Crystal Structure Determinationmentioning

confidence: 99%

Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques

Mazaj

Kaučič

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2016

ACSi

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In the memory of Janez (Janko) Jamnik. AbstractThe research on metal-organic frameworks (MOFs) experienced rapid progress in recent years due to their structure diversity and wide range of application opportunities. Continuous progress of X-ray and neutron diffraction methods enables more and more detailed insight into MOF's structural features and significantly contributes to the understanding of their chemistry. Improved instrumentation and data processing in high-resolution X-ray diffraction methods enables the determination of new complex MOF crystal structures in powdered form. By the use of neutron diffraction techniques, a lot of knowledge about the interaction of guest molecules with crystalline framework has been gained in the past few years. Moreover, in-situ time-resolved studies by various diffraction and scattering techniques provided comprehensive information about crystallization kinetics, crystal growth mechanism and structural dynamics triggered by external physical or chemical stimuli. The review emphasizes most relevant advanced structural studies of MOFs based on powder X-ray and neutron scattering.

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Section: Crystal Structure Determinationmentioning

confidence: 99%

Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques

Mazaj

Kaučič

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2016

ACSi

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“…An ADT data set of a ZSM-5 sample with a similar Si/Al ratio (93.9/2.1) was collected from a broken fragment with the reflections of h00 type missing (Mugnaioli & Kolb, 2013).…”

Section: Zsm-5: Effect Of the Systematic Omission Of Reflections On Tmentioning

confidence: 99%

“…Using this procedure the electron dose on the sample is further reduced, enabling data collection of extremely beam-sensitive materials, like organics and metal-organic frameworks (MOFs) Denysenko et al, 2011;Feyand et al, 2012;Gorelik et al, 2012). ADT is often coupled with precession electron diffraction (PED) (Vincent & Midgley, 1994) to improve the accuracy of the integrated intensities (Mugnaioli et al, 2009) and with cryo-apparatus to increase the stability of samples containing water and organic molecules (Denysenko et al, 2011;Jiang et al, 2011;Feyand et al, 2012;Mugnaioli & Kolb, 2013). Tomographic acquisition has also been complemented in other laboratories with energy filtering (Gemmi & Oleynikov, 2013) and beam tilt (rotation electron diffraction, RED: Zhang et al, 2010).…”

Section: Introductionmentioning

confidence: 99%

“…One peculiarity of the ADT strategy which is inherent to the data-collection geometry is the existence of an experimentally inaccessible part of the reciprocal lattice (hereafter called the missing wedge). In the case of low-symmetry compounds data incompleteness can represent a problem, especially for platelet-like crystals with prominent preferential orientation (Mugnaioli & Kolb, 2013). This is especially true when reflections along principal reciprocal-space directions are missing.…”

Section: Introductionmentioning

confidence: 99%

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Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

et al. 2013

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δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data-collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least-squares refinement have been found. During this study it has been demonstrated that the Wilson-plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.

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“…Beam precession allows the integration of the reflection volume and therefore a significant reduction of the excitation error influence on experimental intensities (Mugnaioli et al 2009a). Actually, PED-ADT intensity data could be used for the structure determination of numerous nanocrystalline phases neglecting dynamical effects and assuming the simple kinematical approximation I hkl -F hkl 2 (see, e.g., Kolb et al 2011;Mugnaioli and Kolb 2013).…”

Section: Introductionmentioning

confidence: 99%

Single nano crystal analysis using automated electron diffraction tomography

Mugnaioli

2014

Rend. Fis. Acc. Lincei

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Most of hitherto unknown natural phases and many new synthetic compounds can grow only in the form of nanocrystals. X-ray powder diffraction is the most widespread technique for the structural characterization of nanomaterials, but its use is limited by two main restrictions: structural information is projected in one dimension and data come from the whole sample and not from a specific single crystallite. On the other hand, crystallographic methods based on the scattering of accelerated electrons are able to obtain 3-D structural data from single volumes of few tens of nanometers. Automated diffraction tomography is a recently developed method able to record more kinematical and complete electron diffraction data. This method consists in the acquisition of a series of electron diffraction patterns while the sample is rotated around an arbitrary tilt axis by sequential mechanical steps, within the full tilt range of the microscope goniometer. Data collection can be performed on highly beam sensitive materials, as no time is required for orienting the crystal along specific crystallographic orientations and mild illumination conditions are used. In the last years many nanocrystalline materials belonging to different material classes have been characterized by automated diffraction tomography. This review describes the different experimental and analytical approaches used for the determination of inorganic and organic phases and points out the advantages offered by automated diffraction tomography for the characterization of minor phases available only in polyphasic nanomixtures and for the description of domain arrangement in polycrystalline nanocomposites.

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Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials

Cited by 37 publications

References 42 publications

Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques

Chemistry of Metal-organic Frameworks Monitored by Advanced X-ray Diffraction and Scattering Techniques

Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

Single nano crystal analysis using automated electron diffraction tomography

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