Browsing by Subject "in situ"

Now showing 1 - 4 of 4
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    Hard X-ray-induced damage on carbon–binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries
    (IUCR, 2017) Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun; Mechanical Engineering, School of Engineering and Technology
    The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment for in situ monitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon–binder matrix by the accumulated X-ray dose is the key factor of radiation damage. For in situ TXM tomography, intermittent X-ray exposure during image capturing can be used to avoid the morphology change caused by radiation damage on the carbon–binder matrix.
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    High temperature phase behavior of 2D transition metal carbides
    (2024-08) Wyatt, Brian C.; Anasori, Babak; Trice, Rodney; Zhang, Jing; Hood, Zachary
    The technological drive of humanity to explore the cosmos, travel at hypersonic speeds, and pursue clean energy solutions requires ceramic scientists and engineers to constantly push materials to their functional, behavioral, and chemical extremes. Ultra-high temperature ceramics, and particularly transition metal carbides, are promising materials to meet the demands of extreme environment materials with their >4000 °C melting temperature and impressive thermomechanical behaviors in extreme conditions. The advent of the 2D version of these transition metal carbides, known as MXenes, added a new direction to design transition metal carbides for energy, catalysis, flexible electronics, and other applications. Toward extreme conditions, although MXenes remain yet unexplored, we believe that the ~1 nm flakes of MXenes gives ceramics scientists and engineers the ability to truly engineer transition metal carbides layer-by-layer at the nanoscale to endure the extreme conditions required by future harsh environment technology. Although MXenes have this inherent promise, fundamental study of their behavior in high-temperature environments is necessary to understand how their chemistry and 2D nature affects the high- temperature stability and phase behavior of MXenes toward application in extreme environments. In this dissertation, we investigate the high-temperature phase behavior of 2D MXenes in high temperature inert environments to understand the stability and phase transition behavior of MXenes. In this work, we demonstrate that 1) MXenes’ transition at high-temperatures is to highly textured transition metal carbides is due to the homoepitaxial growth of these phases onto ~1-nm- thick MXenes’ highly exposed basal plane, 2) the MXene to MXene interface plays a major role in the phase behavior of MXenes, particularly toward building layered transition metal carbides using MXenes as ~1-nm-thick building blocks, and 3) Defects are the primary site at which atomic migration begins during phase transition of MXenes into these highly textured transition metal carbides, and these defects can be engineered for different phase stability of MXenes. To do so, we investigate the phase behavior of Ti3C2Tx, Ta4C3Tx, Mo2TiC2Tx, and other MXenes using a combination of in situ x-ray diffraction and scanning transmission electron microscopy and other ex situ methods, such as secondary ion mass spectrometry and x-ray photoelectron spectroscopy, with other methods. By investigating the fundamentals of the high-temperature phase behavior of MXenes, we hope to establish the basic principles behind use of MXenes as the ideal material for application in future extreme environments.
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    In situ anticaries efficacy of dentifrices with different formulations – A pooled analysis of results from three randomized clinical trials
    (Elsevier, 2018-10) Zero, Domenick T.; Lippert, Frank; Hara, Anderson T.; Creeth, Johnathan; Newby, Evelyn; Butler, Andrew; Constantin, Paul; Bosma, Mary Lynn; Cariology, Operative Dentistry and Dental Public Health, School of Dentistry
    Objectives Data generated from three similar in situ caries crossover studies presented the opportunity to conduct a pooled analysis to investigate how dentifrice formulations with different fluoride salts and combinations at concentrations of 1400–1450 ppm F, different abrasive systems and in some cases, carbomer (Carb), affect enamel caries lesion remineralization and fluoridation. Methods Subjects continuously wore modified partial dentures holding two gauze-covered partially-demineralized human enamel specimens for 14 days and brushed 2×/day with their assigned dentifrice: Study 1: sodium fluoride (NaF)/Carb/silica, NaF/silica, NaF + monofluorophosphate (MFP)/chalk; Study 2: NaF/Carb/silica, NaF + MFP/dical, amine fluoride (AmF)/silica; Study 3: NaF/Carb/silica, NaF + stannous fluoride (SnF2)/silica/hexametaphosphate (HMP). All studies included Placebo (0 ppm F) and/or dose-response controls (675 ppm F as NaF [675F-NaF]) ±Carb. Specimens were evaluated for percentage surface microhardness recovery (SMHR) and enamel fluoride uptake (EFU). Results All 1400–1450 ppm F dentifrices except NaF + SnF2/silica/HMP provided significantly greater lesion remineralization than Placebo (p < 0.0001): differences in SMHR ranged from 17.46% (NaF + MFP/dical) to 26.66% (AmF/silica). For EFU (back-transformed log EFU), all 1400–1450 ppm F dentifrices gave significant fluoride uptake compared to Placebo (p < 0.0001): increases in EFU ranged from 4.95 μg F/cm2 (NaF + SnF2/silica/HMP) to 16.32 μg F/cm2 (NaF/carb/silica). Dentifrices containing NaF or AmF as sole fluoride source provided the greatest remineralization and fluoridation; Carb addition did not alter fluoride efficacy; some excipients appeared to interfere with the cariostatic action of fluoride. Treatments were generally well-tolerated with ≤4 treatment-related adverse events per study. Conclusion Commercially available fluoride dentifrices varied greatly in their ability to remineralize and fluoridate early caries lesions. Clinical significance Fluoride dentifrices are the most impactful anticaries modality worldwide. While clinical caries trials have not consistently shown the superiority of one formulation over another, these findings using a sensitive in situ caries model indicated that dentifrices containing NaF or AmF as the sole fluoride source provided the greatest remineralization and fluoridation benefits.
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    In Situ Focused Ion Beam Scanning Electron Microscope Study of Microstructural Evolution of Single Tin Particle Anode for Li-Ion Batteries
    (ACS, 2019-01) Zhou, Xinwei; Li, Tianyi; Cui, Yi; Fu, Yongzhu; Liu, Yuzi; Zhu, Likun; Mechanical and Energy Engineering, School of Engineering and Technology
    Tin (Sn) is a potential anode material for highenergy density Li-ion batteries because of its high capacity, safety, abundance and low cost. However, Sn suffers from large volume change during cycling, leading to fast degradation of the electrode. For the first time, the microstructural evolution of micrometer-sized single Sn particle was monitored by focused-ion beam (FIB) polishing and scanning electron microscopy (SEM) imaging during electrochemical cycling by in situ FIB-SEM. Our results show the formation and evolution of cracks during lithiation, evolution of porous structure during delithiation and volume expansion/contraction during cycling. The electrochemical performance and the microstructural evolution of the Sn microparticle during cycling are directly correlated, which provides insights for understanding Sn-based electrode materials.