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Condens. Matter 2020, 5, x 3 of 30 Condens. Matter 2020, 5, 75 3 of 28 and symmetry, and the peak intensity is related to the number of atoms and their position within the lattice [24]. Figure 1a shows a scheme of the X-ray diffraction phenomena, with an example of the generated pattern. The diffraction conditions are described by Bragg’s law and expressed in the the generated pattern. The diffraction conditions are described by Bragg’s law and expressed in the scheme where n is an integer related to the plane in which the scattering is originated, d is the distance scheme where n is an integer related to the plane in which the scattering is originated, d is the distance between the crystallographic planes, θ is the half angle between incident and scattered beam, and λ between the crystallographic planes, θ is the half angle between incident and scattered beam, and λ is is the incident X-ray wavelength. the incident X-ray wavelength. Figure 1. (a) schematic of XRD working principle with an example of the obtained pattern; (b) schematic Figure 1. (a) schematic of XRD working principle with an example of the obtained pattern; (b) of the in situ cell developed by Chianelli and co-authors [25]; (c) schematic of the first developed in situ schematic of the in situ cell developed by Chianelli and co-authors [25]; (c) schematic of the first cell for transmission analysis [26]; (d) representation of the in situ cell developed by Amatucci and developed in situ cell for transmission analysis [26]; (d) representation of the in situ cell developed by co-workers [27]. Amatucci and co-workers [27]. An in situ XRD cell has to be designed to satisfy some necessary requirements. Firstly, the cell has An in situ XRD cell has to be designed to satisfy some necessary requirements. Firstly, the cell to allow X-ray penetration, meaning that it must provide an X-ray transparent window, which has to has to allow X-ray penetration, meaning that it must provide an X-ray transparent window, which be also chemically inert and impermeable to oxygen and moisture in order to prevent reaction with has to be also chemically inert and impermeable to oxygen and moisture in order to prevent reaction electrolyte and exposure of the internal materials to air and water; amorphous materials are usually with electrolyte and exposure of the internal materials to air and water; amorphous materials are preferred, since they do not generate a background signal which can contribute to the diffraction pattern. usually preferred, since they do not generate a background signal which can contribute to the Moreover, the cell has to be sealed with materials resistant to any electrolyte leakage or swelling, and the diffraction pattern. Moreover, the cell has to be sealed with materials resistant to any electrolyte two internal electrodes have to be electrically isolated and connected to electrode terminals to complete leakage or swelling, and the two internal electrodes have to be electrically isolated and connected to the circuit and connect to an external potentiostat. Finally, a critical point is a method of compression electrode terminals to complete the circuit and connect to an external potentiostat. Finally, a critical to maintain electrodes in place and improve the cycling performance. Insufficient pressure can lead to point is a method of compression to maintain electrodes in place and improve the cycling the loss of contact between cell parts and therefore limits the electrical conductivity. Uniform stack performance. Insufficient pressure can lead to the loss of contact between cell parts and therefore pressure is essential to avoid heterogeneity in the electrodes under operation, and particularly as the limits the electrical conductivity. Uniform stack pressure is essential to avoid heterogeneity in the location of measurement in many of the techniques mentioned in this review is precisely where the cell electrodes under operation, and particularly as the location of measurement in many of the modifications may lead to the lowest compression of the electrode [28]. techniques mentioned in this review is precisely where the cell modifications may lead to the lowest Generally, for cell windows, materials such as beryllium, glassy carbon, thin polymer films compression of the electrode [28]. such as Kapton tape or Mylar, or thin metal foils, are the most widely applied. Beryllium is the Generally, for cell windows, materials such as beryllium, glassy carbon, thin polymer films such most transparent material to X-rays but is expensive and toxic and is not suitable for high voltage as Kapton tape or Mylar, or thin metal foils, are the most widely applied. Beryllium is the most experiments due to its electrochemical reactivity above 3V [29]. To avoid the high risks related to its transparent material to X-rays but is expensive and toxic and is not suitable for high voltage reactivity, additional layers of conductive materials can be used to prevent direct contact between experiments due to its electrochemical reactivity above 3V [29]. To avoid the high risks related to its electrolyte and beryllium [30,31]. Another approach can be the generation of an air gap between the reactivity, additional layers of conductive materials can be used to prevent direct contact between Be window and the electrochemically active part of the cell, so as to prevent Be reactivity at highPDF Image | Synchrotron-Based X-ray Diffraction for Lithium-Ion Batteries
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