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Targeted Surface Doping with Reversible Local Environment Improves Oxygen Stability at the Electrochemical Interfaces of Nickel-Rich Cathode Materials

Steiner JD, Cheng H, Walsh J, Zhang Y, Zydlewski B, Mu L, et al.

ACS Appl Mater Interfaces, 2019 Oct 16;11(41):37885-37891.
PMID: 31589393 DOI: 10.1021/acsami.9b14729

Elemental doping represents a prominent strategy to improve interfacial chemistry in battery materials. Manipulating the dopant spatial distribution and understanding the dynamic evolution of the dopants at the atomic scale can inform better design of the doping chemistry for batteries. In this work, we create a targeted hierarchical distribution of Ti4+, a popular doping element for oxide cathode materials, in LiNi0.8Mn0.1Co0.1O2 primary particles. We apply multiscale synchrotron/electron spectroscopy and imaging techniques as well as theoretical calculations to investigate the dynamic evolution of the doping chemical environment. The Ti4+ dopant is fully incorporated into the TMO6 octahedral coordination and is targeted to be enriched at the surface. Ti4+ in the TMO6 octahedral coordination increases the TM-O bond length and reduces the covalency between (Ni, Mn, Co) and O. The excellent reversibility of Ti4+ chemical environment gives rise to superior oxygen reversibility at the cathode-electrolyte interphase and in the bulk particles, leading to improved stability in capacity, energy, and voltage. Our work directly probes the chemical environment of doping elements and helps rationalize the doping strategy for high-voltage layered cathodes.

Matched MeSH terms: Synchrotrons
Fulltext Anomalous metal segregation in lithium-rich material provides design rules for stable cathode in lithium-ion battery

Lin R, Hu E, Liu M, Wang Y, Cheng H, Wu J, et al.

Nat Commun, 2019 04 09;10(1):1650.
PMID: 30967531 DOI: 10.1038/s41467-019-09248-0

Despite the importance of studying the instability of delithiated cathode materials, it remains difficult to underpin the degradation mechanism of lithium-rich cathode materials due to the complication of combined chemical and structural evolutions. Herein, we use state-of-the-art electron microscopy tools, in conjunction with synchrotron X-ray techniques and first-principle calculations to study a 4d-element-containing compound, Li2Ru0.5Mn0.5O3. We find surprisingly, after cycling, ruthenium segregates out as metallic nanoclusters on the reconstructed surface. Our calculations show that the unexpected ruthenium metal segregation is due to its thermodynamic insolubility in the oxygen deprived surface. This insolubility can disrupt the reconstructed surface, which explains the formation of a porous structure in this material. This work reveals the importance of studying the thermodynamic stability of the reconstructed film on the cathode materials and offers a theoretical guidance for choosing manganese substituting elements in lithium-rich as well as stoichiometric layer-layer compounds for stabilizing the cathode surface.

Matched MeSH terms: Synchrotrons
Fulltext Influence of Sintering Temperature of Kaolin, Slag, and Fly Ash Geopolymers on the Microstructure, Phase Analysis, and Electrical Conductivity

Zulkifli NNI, Abdullah MMAB, Przybył A, Pietrusiewicz P, Salleh MAAM, Aziz IH, et al.

Materials (Basel), 2021 Apr 26;14(9).
PMID: 33925777 DOI: 10.3390/ma14092213

This paper clarified the microstructural element distribution and electrical conductivity changes of kaolin, fly ash, and slag geopolymer at 900 °C. The surface microstructure analysis showed the development in surface densification within the geopolymer when in contact with sintering temperature. It was found that the electrical conductivity was majorly influenced by the existence of the crystalline phase within the geopolymer sample. The highest electrical conductivity (8.3 × 10-4 Ωm-1) was delivered by slag geopolymer due to the crystalline mineral of gehlenite (3Ca2Al2SiO7). Using synchrotron radiation X-ray fluorescence, the high concentration Ca boundaries revealed the appearance of gehlenite crystallisation, which was believed to contribute to development of denser microstructure and electrical conductivity.

Matched MeSH terms: Synchrotrons
Fulltext Resistance Switching Behavior in Rectangle-Nano-Pattern SrTiO3 Induced by Simple Annealing

Liao X, Zhang Y, Wang J, Kang J, Zhang J, Wang J, et al.

Materials (Basel), 2019 Nov 09;12(22).
PMID: 31717524 DOI: 10.3390/ma12223698

The tunability of semi-conductivity in SrTiO3 single crystal substrates has been realized by a simple encapsulated annealing method under argon atmosphere. This high temperature annealing-induced property changes are characterized by the transmission spectra, scanning electron microscopy (SEM) and synchrotron-based X-ray absorption (XAS). We find the optical property is strongly influenced by the annealing time (with significant decrease of transmittance). A sub gap absorption at ~427 nm is detected which is attributed to the introduction of oxygen vacancy. Interestingly, in the SEM images, annealing-induced regularly rectangle nano-patterns are directly observed which is contributed to the conducting filaments. The XAS of O K-edge spectra shows the changes of electronic structure by annealing. Very importantly, resistance switching response is displayed in the annealed SrTiO3 single crystal. This suggests a possible simplified route to tune the conductivity of SrTiO3 and further develop novel resistance switching materials.

Matched MeSH terms: Synchrotrons
Fulltext Strength Development and Elemental Distribution of Dolomite/Fly Ash Geopolymer Composite under Elevated Temperature

Azimi EA, Abdullah MMAB, Vizureanu P, Salleh MAAM, Sandu AV, Chaiprapa J, et al.

Materials (Basel), 2020 Feb 24;13(4).
PMID: 32102345 DOI: 10.3390/ma13041015

A geopolymer has been reckoned as a rising technology with huge potential for application across the globe. Dolomite refers to a material that can be used raw in producing geopolymers. Nevertheless, dolomite has slow strength development due to its low reactivity as a geopolymer. In this study, dolomite/fly ash (DFA) geopolymer composites were produced with dolomite, fly ash, sodium hydroxide, and liquid sodium silicate. A compression test was carried out on DFA geopolymers to determine the strength of the composite, while a synchrotron Micro-Xray Fluorescence (Micro-XRF) test was performed to assess the elemental distribution in the geopolymer composite. The temperature applied in this study generated promising properties of DFA geopolymers, especially in strength, which displayed increments up to 74.48 MPa as the optimum value. Heat seemed to enhance the strength development of DFA geopolymer composites. The elemental distribution analysis revealed exceptional outcomes for the composites, particularly exposure up to 400 °C, which signified the homogeneity of the DFA composites. Temperatures exceeding 400 °C accelerated the strength development, thus increasing the strength of the DFA composites. This appears to be unique because the strength of ordinary Portland Cement (OPC) and other geopolymers composed of other raw materials is typically either maintained or decreases due to increased heat.

Matched MeSH terms: Synchrotrons
Fulltext Design of next-generation ceramic fuel cells and real-time characterization with synchrotron X-ray diffraction computed tomography

Li T, Heenan TMM, Rabuni MF, Wang B, Farandos NM, Kelsall GH, et al.

Nat Commun, 2019 04 02;10(1):1497.
PMID: 30940801 DOI: 10.1038/s41467-019-09427-z

Ceramic fuel cells offer a clean and efficient means of producing electricity through a variety of fuels. However, miniaturization of cell dimensions for portable device application remains a challenge, as volumetric power densities generated by readily-available planar/tubular ceramic cells are limited. Here, we demonstrate a concept of 'micro-monolithic' ceramic cell design. The mechanical robustness and structural integrity of this design is thoroughly investigated with real-time, synchrotron X-ray diffraction computed tomography, suggesting excellent thermal cycling stability. The successful miniaturization results in an exceptional power density of 1.27 W cm-2 at 800 °C, which is among the highest reported. This holistic design incorporates both mechanical integrity and electrochemical performance, leading to mechanical property enhancement and representing an important step toward commercial development of portable ceramic devices with high volumetric power (>10 W cm-3), fast thermal cycling and marked mechanical reliability.

Matched MeSH terms: Synchrotrons
Fulltext An evaluation of dose equivalence between synchrotron microbeam radiation therapy and conventional broad beam radiation using clonogenic and cell impedance assays

Ibahim MJ, Crosbie JC, Yang Y, Zaitseva M, Stevenson AW, Rogers PA, et al.

PLoS One, 2014;9(6):e100547.
PMID: 24945301 DOI: 10.1371/journal.pone.0100547

High-dose synchrotron microbeam radiation therapy (MRT) has shown the potential to deliver improved outcomes over conventional broadbeam (BB) radiation therapy. To implement synchrotron MRT clinically for cancer treatment, it is necessary to undertake dose equivalence studies to identify MRT doses that give similar outcomes to BB treatments.

Matched MeSH terms: Synchrotrons*
Fulltext Effect of Ni on the Suppression of Sn Whisker Formation in Sn-0.7Cu Solder Joint

Hashim AN, Salleh MAAM, Sandu AV, Ramli MM, Yee KC, Mohd Mokhtar NZ, et al.

Materials (Basel), 2021 Feb 05;14(4).
PMID: 33562471 DOI: 10.3390/ma14040738

The evolution of internal compressive stress from the intermetallic compound (IMC) Cu6Sn5 growth is commonly acknowledged as the key inducement initiating the nucleation and growth of tin (Sn) whisker. This study investigates the effect of Sn-0.7Cu-0.05Ni on the nucleation and growth of Sn whisker under continuous mechanical stress induced. The Sn-0.7Cu-0.05Ni solder joint has a noticeable effect of suppression by diminishing the susceptibility of nucleation and growth of Sn whisker. By using a synchrotron micro X-ray fluorescence (µ-XRF) spectroscopy, it was found that a small amount of Ni alters the microstructure of Cu6Sn5 to form a (Cu,Ni)6Sn5 intermetallic layer. The morphology structure of the (Cu,Ni)6Sn5 interfacial intermetallic layer and Sn whisker growth were investigated by scanning electron microscope (SEM) in secondary and backscattered electron imaging mode, which showed that there is a strong correlation between the formation of Sn whisker and the composition of solder alloy. The thickness of the (Cu,Ni)6Sn5 IMC interfacial layer was relatively thinner and more refined, with a continuous fine scallop-shaped IMC interfacial layer, and consequently enhanced a greater incubation period for the nucleation and growth of the Sn whisker. These verification outcomes proposes a scientifically foundation to mitigate Sn whisker growth in lead-free solder joint.

Matched MeSH terms: Synchrotrons
Fulltext True mechanical behaviour and the associated structure morphology of Poly(Lactid Acid) polymer in strain induced crystallisation by in-situ time resolved x-ray diffraction and scattering technique

Muhammad Rawi Mohamed Zin, Mahendrasingam, Arumugam, Konkel, Chris, Narayanan, Theyencheri

Jurnal Sains Nuklear Malaysia, 2011;23(2):53-59.
MyJurnal

Changes in molecular structure configuration during strain induced crystallisation of an amorphous Poly(Lactic Acid) (PLA 4032D) polymer was monitored in-situ by simultaneously recording the wide angle x-ray scattering (WAXS) and small angle x-ray scattering (SAXS) patterns together with polymer deformation images and force data. The amorphous chain orientation from the beginning of deformation until the onset of crystallisation was studied from the WAXS patterns. The true mechanical behaviour described by the true stress-true strain curve related to an amorphous chain orientation exhibited a linear behaviour. Approaching critical amorphous orientation, the true stress-true strain curve deviated from linear into non-linear behaviour. After the onset of crystallization, when the deformed polymer became a semicrystalline state, the true mechanical behaviour exhibited true strain hardening which greatly affected by the formation of the morphology. The gradual true strain hardening was associated with the formation of micro-fibrillar structure containing thin crystallite morphology whilst sharp increased in true strain hardening was associated with the formation of stacked lamellar morphology in the form of macro-lattice structure. The study was accomplished by the application of high brilliance synchrotron radiation at beamline ID2 of ESRF, Grenoble in France and the usage of the high contrast resolution of WAXS and SAXS charge-couple device (CCD) camera as well as 40 milliseconds temporal resolution of data acquisition system.

Matched MeSH terms: Synchrotrons
Fulltext Quantitative Structural Analysis of Polystyrene Nanoparticles Using Synchrotron X-Ray Scattering and Dynamic Light Scattering

Wong JC, Xiang L, Ngoi KH, Chia CH, Jin KS, Ree M

Polymers (Basel), 2020 Feb 19;12(2).
PMID: 32093008 DOI: 10.3390/polym12020477

A series of polystyrene nanoparticles (PS-1, PS-2, PS-3, and PS-4) in aqueous solutions were investigated in terms of morphological structure, size, and size distribution. Synchrotron small-angle X-ray scattering analysis (SAXS) was carried out, providing morphology details, size and size distribution on the particles. PS-1, PS-2, and PS-3 were confirmed to behave two-phase (core and shell) spherical shapes, whereas PS-4 exhibited a single-phase spherical shape. They all revealed very narrow unimodal size distributions. The structural parameter details including radial density profile were determined. In addition, the presence of surfactant molecules and their assemblies were detected for all particle solutions, which could originate from their surfactant-assisted emulsion polymerizations. In addition, dynamic light scattering (DLS) analysis was performed, finding only meaningful hydrodynamic size and intensity-weighted mean size information on the individual PS solutions because of the particles' spherical nature. In contrast, the size distributions were extracted unrealistically too broad, and the volume- and number-weighted mean sizes were too small, therefore inappropriate to describe the particle systems. Furthermore, the DLS analysis could not detect completely the surfactant and their assemblies present in the particle solutions. Overall, the quantitative SAXS analysis confirmed that the individual PS particle systems were successfully prepared with spherical shape in a very narrow unimodal size distribution.

Matched MeSH terms: Synchrotrons
Fulltext Optimal energy for cell radiosensitivity enhancement by gold nanoparticles using synchrotron-based monoenergetic photon beams

Rahman WN, Corde S, Yagi N, Abdul Aziz SA, Annabell N, Geso M

Int J Nanomedicine, 2014;9:2459-67.
PMID: 24899803 DOI: 10.2147/IJN.S59471

Gold nanoparticles have been shown to enhance radiation doses delivered to biological targets due to the high absorption coefficient of gold atoms, stemming from their high atomic number (Z) and physical density. These properties significantly increase the likelihood of photoelectric effects and Compton scattering interactions. Gold nanoparticles are a novel radiosensitizing agent that can potentially be used to increase the effectiveness of current radiation therapy techniques and improve the diagnosis and treatment of cancer. However, the optimum radiosensitization effect of gold nanoparticles is strongly dependent on photon energy, which theoretically is predicted to occur in the kilovoltage range of energy. In this research, synchrotron-generated monoenergetic X-rays in the 30-100 keV range were used to investigate the energy dependence of radiosensitization by gold nanoparticles and also to determine the photon energy that produces optimum effects. This investigation was conducted using cells in culture to measure dose enhancement. Bovine aortic endothelial cells with and without gold nanoparticles were irradiated with X-rays at energies of 30, 40, 50, 60, 70, 81, and 100 keV. Trypan blue exclusion assays were performed after irradiation to determine cell viability. Cell radiosensitivity enhancement was indicated by the dose enhancement factor which was found to be maximum at 40 keV with a value of 3.47. The dose enhancement factor obtained at other energy levels followed the same direction as the theoretical calculations based on the ratio of the mass energy absorption coefficients of gold and water. This experimental evidence shows that the radiosensitization effect of gold nanoparticles varies with photon energy as predicted from theoretical calculations. However, prediction based on theoretical assumptions is sometimes difficult due to the complexity of biological systems, so further study at the cellular level is required to fully characterize the effects of gold nanoparticles with ionizing radiation.

Matched MeSH terms: Synchrotrons*
Synchrotron microbeam radiotherapy evokes a different early tumor immunomodulatory response to conventional radiotherapy in EMT6.5 mammary tumors

Yang Y, Swierczak A, Ibahim M, Paiva P, Cann L, Stevenson AW, et al.

Radiother Oncol, 2019 04;133:93-99.
PMID: 30935588 DOI: 10.1016/j.radonc.2019.01.006

BACKGROUND: Synchrotron microbeam radiation therapy (MRT) is a new, evolving form of radiotherapy that has potential for clinical application. Several studies have shown in preclinical models that synchrotron MRT achieves equivalent tumor control to conventional radiotherapy (CRT) but with significantly reduced normal tissue damage.
METHODS: To explore differences between these two modalities, we assessed the immune cell infiltrate into EMT6.5 mammary tumors after CRT and MRT.
RESULTS: CRT induced marked increases in tumor-associated macrophages and neutrophils while there were no increases in these populations following MRT. In contrast, there were higher numbers of T cells in the MRT treated tumors. There were also increased levels of CCL2 by immunohistochemistry in tumors subjected to CRT, but not to MRT. Conversely, we found that MRT induced higher levels of pro-inflammatory genes in tumors than CRT.
CONCLUSION: Our data are the first to demonstrate substantial differences in macrophage, neutrophil and T cell numbers in tumors following MRT versus CRT, providing support for the concept that MRT evokes a different immunomodulatory response in tumors compared to CRT.

Matched MeSH terms: Synchrotrons
Eosinophil-Associated Gene Pathways but not Eosinophil Numbers are Differentially Regulated between Synchrotron Microbeam Radiation Treatment and Synchrotron Broad-Beam Treatment by 48 Hours Postirradiation

Ibahim MJ, Yang Y, Crosbie JC, Stevenson A, Cann L, Paiva P, et al.

Radiat Res, 2016 Jan;185(1):60-8.
PMID: 26720800 DOI: 10.1667/RR14115.1

Synchrotron microbeam radiation treatment (MRT) is a preclinical radiotherapy technique with considerable clinical promise, although some of the underlying radiobiology of MRT is still not well understood. In recently reported studies, it has been suggested that MRT elicits a different tumor immune profile compared to broad-beam treatment (BB). The aim of this study was to investigate the effects of synchrotron MRT and BB on eosinophil-associated gene pathways and eosinophil numbers within and around the tumor in the acute stage, 48 h postirradiation. Balb/C mice were inoculated with EMT6.5 mouse mammary tumors and irradiated with microbeam radiation (112 and 560 Gy) and broad-beam radiation (5 and 9 Gy) at equivalent doses determined from a previous in vitro study. After tumors were collected 24 and 48 h postirradiation, RNA was extracted and quantitative PCR performed to assess eosinophil-associated gene expression. Immunohistochemistry was performed to detect two known markers of eosinophils: eosinophil-associated ribonucleases (EARs) and eosinophil major basic protein (MBP). We identified five genes associated with eosinophil function and recruitment (Ear11, Ccl24, Ccl6, Ccl9 and Ccl11) and all of them, except Ccl11, were differentially regulated in synchrotron microbeam-irradiated tumors compared to broad-beam-irradiated tumors. However, immunohistochemical localization demonstrated no significant differences in the number of EAR- and MBP-positive eosinophils infiltrating the primary tumor after MRT compared to BB. In conclusion, our work demonstrates that the effects of MRT on eosinophil-related gene pathways are different from broad-beam radiation treatment at doses previously demonstrated to be equivalent in an in vitro study. However, a comparison of the microenvironments of tumors, which received MRT and BB, 48 h after exposure showed no difference between them with respect to eosinophil accumulation. These findings contribute to our understanding of the role of differential effects of MRT on the tumor immune response.

Matched MeSH terms: Synchrotrons
Fulltext Structural Studies of Epithelial Mesenchymal Transition Breast Tissues

Mohd Sobri SN, Abdul Sani SF, Sabtu SN, Looi LM, Chiew SF, Pathmanathan D, et al.

Sci Rep, 2020 02 06;10(1):1997.
PMID: 32029810 DOI: 10.1038/s41598-020-58932-5

At the supramolecular level, the proliferation of invasive ductal carcinoma through breast tissue is beyond the range of standard histopathology identification. Using synchrotron small angle x-ray scattering (SAXS) techniques, determining nanometer scale structural changes in breast tissue has been demonstrated to allow discrimination between different tissue types. From a total of 22 patients undergoing symptomatic investigations, different category breast tissue samples were obtained in use of surgically removed tissue, including non-lesional, benign and malignant tumour. Structural components of the tissues were examined at momentum transfer values between q = 0.2 nm-1 and 1.5 nm-1. From the SAXS patterns, axial d-spacing and diffuse scattering intensity were observed to provide the greatest discrimination between the various tissue types, specifically in regard to the epithelial mesenchymal transition (EMT) structural component in malignant tissue. In non-lesional tissue the axial period of collagen is within the range 63.6-63.7 nm (formalin fixed paraffin embedded (FFPE) dewaxed) and 63.4 (formalin fixed), being 0.9 nm smaller than in EMT cancer-invaded regions. The overall intensity of scattering from cancerous regions is a degree of magnitude greater in cancer-invaded regions. Present work has found that the d-spacing of the EMT positive breast cancer tissue (FFPE (dewaxed)) is within the range 64.5-64.7 nm corresponding to the 9th and 10th order peaks. Of particular note in regard to formalin fixation of samples is that no alteration is observed to occur in the relative differences in collagen d-spacing between non-lesional and malignant tissues. This is a matter of great importance given that preserved-sample and also retrospective study of samples is greatly facilitated by formalin fixation. Present results indicate that as aids in tissue diagnosis SAXS is capable of distinguishing areas of invasion by disease as well as delivering further information at the supramolecular level.

Matched MeSH terms: Synchrotrons

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