Search Results

You searched for all publications:

with publication states 'Published (Approved)'

Search Again...

These results only include publications that have been reviewed and processed by Diamond Light Source. To also view papers that have not yet been processed click here.

You can use the folder icon under Actions to collate papers as required. You can then click on View Folder in the left-hand navigation to review and/or download your folder.

Exact matches
Related results

36 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I13-1-Coherence	Dual energy X-ray beam ptycho-fluorescence imaging Silvia Cipiccia , Francesco Brun , Vittorio Di Trapani , Christoph Rau , Darren J. Batey Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521008675 Diamond Proposal Number(s): [21767] Open Access Show Abstract ▼ Abstract: X-ray ptychography and X-ray fluorescence are complementary nanoscale imaging techniques, providing structural and elemental information, respectively. Both methods acquire data by scanning a localized beam across the sample. X-ray ptychography processes the transmission signal of a coherent illumination interacting with the sample, to produce images with a resolution finer than the illumination spot and step size. By enlarging both the spot and the step size, the technique can cover extended regions efficiently. X-ray fluorescence records the emitted spectra as the sample is scanned through the localized beam and its spatial resolution is limited by the spot and step size. The requisites for fast ptychography and high-resolution fluorescence appear incompatible. Here, a novel scheme that mitigates the difference in requirements is proposed. The method makes use of two probes of different sizes at the sample, generated by using two different energies for the probes and chromatic focusing optics. The different probe sizes allow to reduce the number of acquisition steps for the joint fluorescence–ptychography scan compared with a standard single beam scan, while imaging the same field of view. The new method is demonstrated experimentally using two undulator harmonics, a Fresnel zone plate and an energy discriminating photon counting detector.	Nov 2021
I13-1-Coherence	Hard x-ray nanotomography for 3D analysis of coking in nickel-based catalysts Sebastian Weber , Darren Batey , Silvia Cipiccia , Matthias Stehle , Ken L. Abel , Roger Gläser , Thomas Lennon Sheppard Angewandte Chemie International Edition DOI: 10.1002/anie.202106380 Diamond Proposal Number(s): [24079] Open Access Show Abstract ▼ Abstract: Understanding catalyst deactivation by coking is crucial for knowledge-based catalyst and process design in reactions with carbonaceous species. Post-mortem analysis of catalyst coking is often performed by bulk characterization methods. Here hard X-ray ptychographic computed tomography (PXCT) was used to study Ni/Al2O3 catalysts for CO2 methanation and CH4 dry reforming after artificial coking treatment. PXCT generated quantitative 3D maps of local electron density at ca. 80 nm resolution, allowing to visualize and evaluate the severity of coking in entire catalyst particles of ca. 40 µm diameter. Coking was primarily revealed in the nanoporous solid, which was not detectable in resolved macropores. Coke formation was independently confirmed by operando Raman spectroscopy. PXCT is highlighted as an emerging characterization tool for nanoscale identification, co-localization, and potentially quantification of deactivation phenomena in 3D space within entire catalyst particles.	Aug 2021
I13-1-Coherence	Imaging defects in vanadium( iii ) oxide nanocrystals using Bragg coherent diffractive imaging Zachary Barringer , Jie Jiang , Xiaowen Shi , Elijah Schold , Anastasios Pateras , Silvia Cipiccia , Christoph Rau , Jian Shi , Edwin Fohtung Crystengcomm 54 DOI: 10.1039/D1CE00736J Diamond Proposal Number(s): [20381] Show Abstract ▼ Abstract: Defects in strongly correlated materials such as V2O3 play influential roles on their electrical properties. Understanding the defects' structure is of paramount importance. In this project, we investigate defect structures in V2O3 grown via a flux method. We use AFM to see surface features in several large flake-like particles that exhibit characteristics of spiral growth. We also use Bragg coherent diffractive imaging (BCDI) to probe in 3 dimensions a smaller particle without flake-like morphology and note an absence of the pure screw dislocation characteristic of spiral growth. We identified and measured several defects by comparing the observed local displacement of the crystal, measured via BCDI to well-known models of the displacement around defects in the crystal. We identified two image file: d1ce00736j-t1.tif partial dislocations in the crystal. We discuss how defects of different types influence the morphology of V2O3 crystals grown via a flux method.	Jul 2021
I13-1-Coherence	X-ray ptychography with a laboratory source Darren Batey , Frederic Van Assche , Sander Vanheule , Matthieu N. Boone , Andrew J. Parnell , Oleksandr O. Mykhaylyk , Christoph Rau , Silvia Cipiccia Physical Review Letters 126 DOI: 10.1103/PhysRevLett.126.193902 Open Access Show Abstract ▼ Abstract: X-ray ptychography has revolutionized nanoscale phase contrast imaging at large-scale synchrotron sources in recent years. We present here the first successful demonstration of the technique in a small-scale laboratory setting. An experiment was conducted with a liquid metal-jet x-ray source and a single photon-counting detector with a high spectral resolution. The experiment used a spot size of 5 μ m to produce a ptychographic phase image of a Siemens star test pattern with a submicron spatial resolution. The result and methodology presented show how high-resolution phase contrast imaging can now be performed at small-scale laboratory sources worldwide.	May 2021
I13-1-Coherence	X-ray ptychography imaging of human chromosomes after low-dose irradiation Archana Bhartiya , Darren Batey , Silvia Cipiccia , Xiaowen Shi , Christoph Rau , Stanley Botchway , Mohammed Yusuf , Ian K. Robinson Chromosome Research 55 DOI: 10.1007/s10577-021-09660-7 Open Access Show Abstract ▼ Abstract: Studies of the structural and functional role of chromosomes in cytogenetics have spanned more than 10 decades. In this work, we take advantage of the coherent X-rays available at the latest synchrotron sources to extract the individual masses of all 46 chromosomes of metaphase human B and T cells using hard X-ray ptychography. We have produced ‘X-ray karyotypes’ of both heavy metal–stained and unstained spreads to determine the gain or loss of genetic material upon low-level X-ray irradiation doses due to radiation damage. The experiments were performed at the I-13 beamline, Diamond Light Source, Didcot, UK, using the phase-sensitive X-ray ptychography method.	Mar 2021
I13-1-Coherence	Operando Bragg coherent diffraction imaging of LiNi0.8Mn0.1Co0.1O2 primary particles within commercially printed NMC811 electrode sheets Ana Katrina C. Estandarte , Jiecheng Diao , Alice Llewellyn , Anmol Jnawali , Thomas M. M. Heenan , Sohrab R. Daemi , Josh J. Bailey , Silvia Cipiccia , Darren Batey , Xiaowen Shi , Christoph Rau , Dan J. L. Brett , Rhodri Jervis , Ian K. Robinson , Paul Shearing Acs Nano DOI: 10.1021/acsnano.0c08575 Diamond Proposal Number(s): [25852, 25440, 24129, 22373, 22309, 21652] Show Abstract ▼ Abstract: Due to complex degradation mechanisms, disparities between the theoretical and practical capacities of lithium-ion battery cathode materials persist. Specifically, Ni-rich chemistries such as LiNi0.8Mn0.1Co0.1O2 (or NMC811) are one of the most promising choices for automotive applications; however, they continue to suffer severe degradation during operation that is poorly understood, thus challenging to mitigate. Here we use operando Bragg coherent diffraction imaging for 4D analysis of these mechanisms by inspecting the individual crystals within primary particles at various states of charge (SoC). Although some crystals were relatively homogeneous, we consistently observed non-uniform distributions of inter- and intracrystal strain at all measured SoC. Pristine structures may already possess heterogeneities capable of triggering crystal splitting and subsequently particle cracking. During low-voltage charging (2.7–3.5 V), crystal splitting may still occur even during minimal bulk deintercalation activity; and during discharging, rotational effects within parallel domains appear to be the precursor for the nucleation of screw dislocations at the crystal core. Ultimately, this discovery of the central role of crystal grain splitting in the charge/discharge dynamics may have ramifications across length scales that affect macroscopic performance loss during real-world battery operation.	Dec 2020
I13-1-Coherence I18-Microfocus Spectroscopy	Structural and compositional characteristics of Fukushima release particulate material from Units 1 and 3 elucidates release mechanisms, accident chronology and future decommissioning strategy Peter Martin , Christopher P. Jones , Stuart Bartlett , Konstantin Ignatyev , Dave Megson-Smith , Yukihiko Sato , Silvia Cipiccia , Darren J. Batey , Christoph Rau , Keisuke Sueki , Tatsuya Ishii , Junya Igarashi , Kazuhiko Ninomiya , Atsushi Shinohara , Alison Rust , Thomas B. Scott Scientific Reports 10 DOI: 10.1038/s41598-020-79169-2 Diamond Proposal Number(s): [24769, 19881] Open Access Show Abstract ▼ Abstract: The structural form and elemental distribution of material originating from different Fukushima Daiichi Nuclear Power Plant reactors (Units 1 and 3) is hereby examined to elucidate their contrasting release dynamics and the current in-reactor conditions to influence future decommissioning challenges. Complimentary computed X-ray absorption tomography and X-ray fluorescence data show that the two suites of Si-based material sourced from the different reactor Units have contrasting internal structure and compositional distribution. The known event and condition chronology correlate with the observed internal and external structures of the particulates examined, which suggest that Unit 1 ejecta material sustained a greater degree of melting than that likely derived from reactor Unit 3. In particular, we attribute the near-spherical shape of Unit 1 ejecta and their internal voids to there being sufficient time for surface tension to round these objects before the hot (and so relatively low viscosity) silicate melt cooled to form glass. In contrast, a more complex internal form associated with the sub-mm particulates invoked to originate from Unit 3 suggest a lower peak temperature, over a longer duration. Using volcanic analogues, we consider the structural form of this material and how it relates to its environmental particulate stability and the bulk removal of residual materials from the damaged reactors. We conclude that the brittle and angular Unit 3 particulate are more susceptible to further fragmentation and particulate generation hazard than the round, higher-strength, more homogenous Unit 1 material.	Dec 2020
I13-1-Coherence	Porosity and structure of hierarchically porous Ni/Al2O3 catalysts for CO2 methanation Sebastian Weber , Ken L. Abel , Ronny T. Zimmermann , Xiaohui Huang , Jens Bremer , Liisa K. Rihko-Struckmann , Darren Batey , Silvia Cipiccia , Juliane Titus , David Poppitz , Christian Kübel , Kai Sundmacher , Roger Gläser , Thomas L. Sheppard Catalysts 10 DOI: 10.3390/catal10121471 Diamond Proposal Number(s): [24079] Open Access Show Abstract ▼ Abstract: CO2 methanation is often performed on Ni/Al2O3 catalysts, which can suffer from mass transport limitations and, therefore, decreased efficiency. Here we show the application of a hierarchically porous Ni/Al2O3 catalyst for methanation of CO2. The material has a well-defined and connected meso- and macropore structure with a total porosity of 78%. The pore structure was thoroughly studied with conventional methods, i.e., N2 sorption, Hg porosimetry, and He pycnometry, and advanced imaging techniques, i.e., electron tomography and ptychographic X-ray computed tomography. Tomography can quantify the pore system in a manner that is not possible using conventional porosimetry. Macrokinetic simulations were performed based on the measures obtained by porosity analysis. These show the potential benefit of enhanced mass-transfer properties of the hierarchical pore system compared to a pure mesoporous catalyst at industrially relevant conditions. Besides the investigation of the pore system, the catalyst was studied by Rietveld refinement, diffuse reflectance ultraviolet-visible (DRUV/vis) spectroscopy, and H2-temperature programmed reduction (TPR), showing a high reduction temperature required for activation due to structural incorporation of Ni into the transition alumina. The reduced hierarchically porous Ni/Al2O3 catalyst is highly active in CO2 methanation, showing comparable conversion and selectivity for CH4 to an industrial reference catalyst.	Dec 2020
I13-1-Coherence I13-2-Diamond Manchester Imaging	Multiscale characterization of the 3D network structure of metal carbides in a Ni superalloy by synchrotron X-ray microtomography and ptychography Zhiguo Zhang , Jia Chuan Khong , Billy Koe , Shifeng Luo , Shi Huang , Ling Qin , Silvia Cipiccia , Darren Batey , Andrew J. Bodey , Christoph Rau , Yu Lung Chiu , Zhu Zhang , Jean-Christophe Gebelin , Nick Green , Jiawei Mi Scripta Materialia 193, 71 - 76 DOI: 10.1016/j.scriptamat.2020.10.032 Diamond Proposal Number(s): [9974, 13488, 22525] Open Access Show Abstract ▼ Abstract: Synchrotron X-ray microtomography and ptychography were used to characterize the 3D network structure, morphology and distribution of metal carbides in an as-cast IN713LC Ni superalloy. MC typed carbides were found to distribute mainly on the grain boundary between the matrix γ and γ' phase. The differences in solidification cooling rate had a minor influence on the volume fraction of the MC type carbides, but significantly affected the carbide size, distribution and network morphology. Depending on the local composition of the remaining liquid phase and geometric constraints, the carbides can form either spherical or strip or network morphologies. The research demonstrated clearly the advantage and technical potential of using the two complementary tomography techniques synergistically to characterize non-destructively complex multiple-phase structures in three dimensional space with a spatial resolution of ~30 nm.	Oct 2020
I13-1-Coherence	Evolution of ferroelastic domain walls during phase transitions in barium titanate nanoparticles Jiecheng Diao , Xiaowen Shi , Tadesse A. Assefa , Longlong Wu , Ana F. Suzana , Daniel S. Nunes , Darren Batey , Silvia Cipiccia , Christoph Rau , Ross J. Harder , Wonsuk Cha , Ian K. Robinson Physical Review Materials 4 DOI: 10.1103/PhysRevMaterials.4.106001 Show Abstract ▼ Abstract: In this work, ferroelastic domain walls inside BaTiO 3 (BTO) tetragonal nanocrystals are distinguished by Bragg peak position and studied with Bragg coherent x-ray diffraction imaging (BCDI). Convergence-related features of the BCDI method for strongly phased objects are reported. A ferroelastic domain wall inside a BTO crystal has been tracked and imaged across the tetragonal-cubic phase transition and proves to be reversible. The linear relationship of relative displacement between two twin domains with temperature is measured and shows a different slope for heating and cooling, while the tetragonality reproduces well over temperature changes in both directions. An edge dislocation is also observed and found to annihilate when heating the crystal close to the phase transition temperature.	Oct 2020

Publications Database

Search Results

You searched for all publications:

Search Again...

Subject Areas (check all that apply) select all

Instruments used to collect data (check all that apply) select all

Collaborations involved (check all that apply) select all

Diamond Offline Facilities used

Relevant Technical Areas (check all that apply) select all

Menu for Anonymous User