scholarly journals In Situ and In Operando Techniques to Study Li-Ion and Solid-State Batteries: Micro to Atomic Level

Inorganics ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 85
Author(s):  
Maryam Golozar ◽  
Raynald Gauvin ◽  
Karim Zaghib
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Atomic Level ◽  
X Ray ◽  
In Situ Techniques ◽  
Transmission Electron ◽  
Wide Range ◽  
Li Ion

This work summarizes the most commonly used in situ techniques for the study of Li-ion batteries from the micro to the atomic level. In situ analysis has attracted a great deal of interest owing to its ability to provide a wide range of information about the cycling behavior of batteries from the beginning until the end of cycling. The in situ techniques that are covered are: X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Scanning Transmission Electron Microscopy (STEM). An optimized setup is required to be able to use any of these in situ techniques in battery applications. Depending on the type of data required, the available setup, and the type of battery, more than one of these techniques might be needed. This study organizes these techniques from the micro to the atomic level, and shows the types of data that can be obtained using these techniques, their advantages and their challenges, and possible strategies for overcoming these challenges.

scholarly journals 3D Modeling of Silver Doped ZrO2 Coupled Graphene-Based Mesoporous Silica Quaternary Nanocomposite for a Nonenzymatic Glucose Sensing Effects

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 193
Author(s):  
Kamrun Nahar Fatema ◽  
Chang-Sung Lim ◽  
Yin Liu ◽  
Kwang-Youn Cho ◽  
Chong-Hun Jung ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Mesoporous Silica ◽  
Photoelectron Spectroscopy ◽  
Glucose Sensor ◽  
Diffuse Reflectance Spectroscopy ◽  
Active Material ◽  
Glucose Sensing ◽  
X Ray ◽  
Transmission Electron

We described the novel nanocomposite of silver doped ZrO2 combined graphene-based mesoporous silica (ZrO2-Ag-G-SiO2,) in bases of low-cost and self-assembly strategy. Synthesized ZrO2-Ag-G-SiO2 were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, Nitrogen adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS), and Diffuse Reflectance Spectroscopy (DRS). The ZrO2-Ag-G-SiO2 as an enzyme-free glucose sensor active material toward coordinate electro-oxidation of glucose was considered through cyclic voltammetry in significant electrolytes, such as phosphate buffer (PBS) at pH 7.4 and commercial urine. Utilizing ZrO2-Ag-G-SiO2, glucose detecting may well be finished with effective electrocatalytic performance toward organically important concentrations with the current reaction of 9.0 × 10−3 mAcm−2 and 0.05 mmol/L at the lowest potential of +0.2 V, thus fulfilling the elemental prerequisites for glucose detecting within the urine. Likewise, the ZrO2-Ag-G-SiO2 electrode can be worked for glucose detecting within the interferometer substances (e.g., ascorbic corrosive, lactose, fructose, and starch) in urine at proper pH conditions. Our results highlight the potential usages for qualitative and quantitative electrochemical investigation of glucose through the ZrO2-Ag-G-SiO2 sensor for glucose detecting within the urine concentration.

scholarly journals Amorphous Ni x Co y P-supported TiO2 nanotube arrays as an efficient hydrogen evolution reaction electrocatalyst in acidic solution

2019 ◽  
Vol 10 ◽  
pp. 62-70 ◽  
Author(s):  
Yong Li ◽  
Peng Yang ◽  
Bin Wang ◽  
Zhongqing Liu
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Hydrogen Evolution ◽  
Hydrogen Evolution Reaction ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Nanotube Arrays ◽  
Active Surface Area ◽  
X Ray ◽  
Transmission Electron

Bimetallic phosphides have been attracting increasing attention due to their synergistic effect for improving the hydrogen evolution reaction as compared to monometallic phosphides. In this work, NiCoP modified hybrid electrodes were fabricated by a one-step electrodeposition process with TiO2 nanotube arrays (TNAs) as a carrier. X-ray diffraction, transmission electron microscopy, UV–vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy and scanning transmission electron microscopy/energy-dispersive X-ray spectroscopy were used to characterize the physiochemical properties of the samples. The electrochemical performance was investigated by cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy. We show that after incorporating Co into Ni–P, the resulting Ni x Co y P/TNAs present enhanced electrocatalytic activity due to the improved electron transfer and increased electrochemically active surface area (ECSA). In 0.5 mol L−1 H2SO4 electrolyte, the Ni x Co y P/TNAs (x = 3.84, y = 0.78) demonstrated an ECSA value of 52.1 mF cm−2, which is 3.8 times that of Ni–P/TNAs (13.7 mF cm−2). In a two-electrode system with a Pt sheet as the anode, the Ni x Co y P/TNAs presented a bath voltage of 1.92 V at 100 mA cm−2, which is an improvment of 79% over that of 1.07 V at 10 mA cm−2.

scholarly journals Synthesis of nickel/gallium nanoalloys using a dual-source approach in 1-alkyl-3-methylimidazole ionic liquids

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dual Source ◽  
Induced Decomposition

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.

Limitations to the use of Sb as a Surfactant During SiGe MBE

1998 ◽  
Vol 533 ◽  
Author(s):  
Glenn G. Jernigan ◽  
Conrad L. Silvestre ◽  
Mohammad Fatemi ◽  
Mark E. Twigg ◽  
Phillip E. Thompson
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Quantum Well ◽  
Photoelectron Spectroscopy ◽  
Surface Coverage ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Alloy Concentration

AbstractThe use of Sb as a surfactant in suppressing Ge segregation during SiGe alloy growth was investigated as a function of Sb surface coverage, Ge alloy concentration, and alloy thickness using xray photoelectron spectroscopy, x-ray diffraction, and transmission electron microscopy. Unlike previous studies where Sb was found to completely quench Ge segregation into a Si capping layer, we find that Sb can not completely prevent Ge segregation while Si and Ge are being co-deposited. This results in the production of a non-square quantum well with missing Ge at the beginning and extra Ge at the end of the alloy. We also found that Sb does not relieve strain in thin films but does result in compositional or strain variations within thick alloy layers.

scholarly journals Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens

2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
General Procedure ◽  
Ion Beam ◽  
Metals And Alloys ◽  
Stainless Steel Sample ◽  
Transmission Electron ◽  
Wide Range

AbstractIn recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

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