Fast-ADT: A fast and automated electron diffraction tomography setup for structure determination and refinement

Plana-Ruiz, Sergi; Krysiak, Yaşar; Portillo, J.; Alig, Edith; Estradé, S.; Peiró, Francesca; Kolb, Ute

doi:10.1016/j.ultramic.2020.112951

Cited by 62 publications

(64 citation statements)

References 65 publications

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“…http://www.minsocam.org/ fortunately found at the nanoscale, partially covered by francevillite (Fig. 3), from which PEDT data could be recorded at 100 K. For each selected crystal area, a series of non-oriented patterns are sequentially collected by step of 1° on the accessible tilt range of the goniometer automated by the in-house software, including the tracking of the crystal following the procedure described by Plana-Ruiz et al (2020) and Kolb et al (2019). The data reduction was performed using the computer programs PETS2 (Palatinus et al 2019).…”

Section: D Ed Data Collectionmentioning

confidence: 99%

Uranotungstite, the only natural uranyl tungstate: Crystal structure revealed from 3D electron diffraction

Steciuk,

Kolitsch,

Goliáš

et al. 2022

American Mineralogist

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Uranotungstite is an uranyl-tungstate mineral that was until recently only partially characterized with a formula originally given as (Fe 2+ ,Ba,Pb)(UO 2 ) 2 (WO 4 )(OH) 4 •12H 2 O and an unknown crystal structure. This mineral has been reinvestigated by electron microprobe analysis coupled with 3D electron diffraction. According to the electron microprobe data, the holotype material from the Menzenschwand uranium deposit (Black Forest, Germany) has the empirical formula (Ba 0.35 Pb 0.27 ) Σ0.62 [(U 6+ O 2 ) 2 (W 6+ 0.98 Fe 3+ 0.26 □ 0.75 )O 4.7 (OH) 2.5 (H 2 O) 1.75 ](H 2 O) 1.67

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Section: D Ed Data Collectionmentioning

confidence: 99%

Uranotungstite, the only natural uranyl tungstate: Crystal structure revealed from 3D electron diffraction

Steciuk,

Kolitsch,

Goliáš

et al. 2022

American Mineralogist

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“…Thus, our data showed it was possible to acquire the necessary dataset for the determination of the spinel content present in the crystal without observably affecting it during at least 60 min, using normal electron diffraction settings. A manually obtained 3D ED series takes less than 60 min, and automated ones take only a few minutes [35][36][37][38][39], while an in zone PED pattern takes mainly the time necessary to orient the pattern. Therefore, 3D ED series and in-zone PED patterns can be obtained without affecting the spinel content.…”

Section: Effect Of the Electron Beam On The Spinel Ratio In Lr-nmc Battery Cathode Materials When Using Electron Diffractionmentioning

confidence: 99%

Determination of Spinel Content in Cycled Li1.2Ni0.13Mn0.54Co0.13O2 Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction

et al. 2021

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Among lithium battery cathode materials, Li1.2Ni0.13Mn0.54Co0.13O2 (LR-NMC) has a high theoretical capacity, but suffers from voltage and capacity fade during cycling. This is partially ascribed to transition metal cation migration, which involves the local transformation of the honeycomb layered structure to spinel-like nano-domains. Determination of the honeycomb layered/spinel phase ratio from powder X-ray diffraction data is hindered by the nanoscale of the functional material and the domains, diverse types of twinning, stacking faults, and the possible presence of the rock salt phase. Determining the phase ratio from transmission electron microscopy imaging can only be done for thin regions near the surfaces of the crystals, and the intense beam that is needed for imaging induces the same transformation to spinel as cycling does. In this article, it is demonstrated that the low electron dose sufficient for electron diffraction allows the collection of data without inducing a phase transformation. Using calculated electron diffraction patterns, we demonstrate that it is possible to determine the volume ratio of the different phases in the particles using a pair-wise comparison of the intensities of the reflections. Using this method, the volume ratio of spinel structure to honeycomb layered structure is determined for a submicron sized crystal from experimental three-dimensional electron diffraction (3D ED) and precession electron diffraction (PED) data. Both twinning and the possible presence of the rock salt phase are taken into account. After 150 charge–discharge cycles, 4% of the volume in LR-NMC particles was transformed irreversibly from the honeycomb layered structure to the spinel structure. The proposed method would be applicable to other multi-phase materials as well.

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“…[1][2][3][4] The early development of 3DED techniques such as ADT/PEDT, 5,6 RED, 7,8 and EDT 9 utilize stepwise rotation, where a crystal is tilted along an arbitrary axis in a transmission electron microscope (TEM), and electron diffraction (ED) patterns are collected at each angle. Recently, new protocols of 3DED, such as continuous rotation electron diffraction (cRED), 10 fast ADT/EDT, 11,12 microED, 13 and rotation electron diffraction, 14 have been developed. They are based on continuous data acquisition where the goniometer continuously rotates at a constant speed and the detector records a movie of ED patterns.…”

Section: Introductionmentioning

confidence: 99%

On the completeness of three-dimensional electron diffraction data for structural analysis of metal–organic frameworks

et al. 2021

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Fast-ADT: A fast and automated electron diffraction tomography setup for structure determination and refinement

Cited by 62 publications

References 65 publications

Uranotungstite, the only natural uranyl tungstate: Crystal structure revealed from 3D electron diffraction

Uranotungstite, the only natural uranyl tungstate: Crystal structure revealed from 3D electron diffraction

Determination of Spinel Content in Cycled Li1.2Ni0.13Mn0.54Co0.13O2 Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction

On the completeness of three-dimensional electron diffraction data for structural analysis of metal–organic frameworks

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