An electrochemical cell for operando bench-top X-ray diffraction

2019 ◽  
Vol 52 (2) ◽  
pp. 485-490 ◽  
Author(s):  
Jonas Sottmann ◽  
Valérie Pralong ◽  
Nicolas Barrier ◽  
Christine Martin

An X-ray transparent electrochemical cell for operando bench-top X-ray diffraction in reflection geometry is presented. Dense glassy carbon (Sigradur-G) is used as an X-ray transparent window. The cell and dedicated sample holder are easy to handle and cost efficient thanks to their simple designs. To demonstrate the performance of this new Swagelok-type operando cell, diffractograms were collected during cycling of the cathode material Li x Mn2O4 (x ≤ 1) in a lithium-ion battery. During charging/delithiation, three spinel phases with evolving lattice parameters were found. This observation confirms the expected mixed two-phase and solid-solution behaviour and thereby validates our experimental setup. The presented low-cost setup may enable further battery research units to access operando X-ray diffraction data for characterization of structural phenomena during battery cycling and degradation mechanisms during prolonged cycling, which will lead to improvement of the battery technology.

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3502
Author(s):  
Fangzhou Song ◽  
Masayoshi Uematsu ◽  
Takeshi Yabutsuka ◽  
Takeshi Yao ◽  
Shigeomi Takai

LATP-based composite electrolytes were prepared by sintering the mixtures of LATP precursor and La2O3 nano-powder. Powder X-ray diffraction and scanning electron microscopy suggest that La2O3 can react with LATP during sintering to form fine LaPO4 particles that are dispersed in the LATP matrix. The room temperature conductivity initially increases with La2O3 nano-powder addition showing the maximum of 0.69 mS∙cm−1 at 6 wt.%, above which, conductivity decreases with the introduction of La2O3. The activation energy of conductivity is not largely varied with the La2O3 content, suggesting that the conduction mechanism is essentially preserved despite LaPO4 dispersion. In comparison with the previously reported LATP-LLTO system, although some unidentified impurity slightly reduces the conductivity maximum, the fine dispersion of LaPO4 particles can be achieved in the LATP–La2O3 system.


Author(s):  
Adelyna Oktavia ◽  
Kurnia Sembiring ◽  
Slamet Priyono

Hospho-material of olivine, LiMnPO4 identified as promising for cathode material generation next Lithium-ion battery and has been successfully synthesized by solid-state method with Li2Co3, 2MnO2, 2NH4H2PO4 as raw material. The influence of initial concentration of precursors at kalsinasi temperatures (400-800 ° C) flows with nitrogen. The purity and composition phase verified by x-ray diffraction analysis (XRD), scanning electron microscopy (SEM), spectroscopy, energy Dispersive x-ray Analysis (EDS), Raman spectra. General investigation shows that there is a correlation between the concentration of precursors, the temperature and the temperature of sintering kalsinasi that can be exploited to design lithium-ion next generation.


2014 ◽  
Vol 895 ◽  
pp. 147-150 ◽  
Author(s):  
Nur Ain Ibrahim ◽  
Noriean Azraaie ◽  
Nurul Aimi Mohd Zainul Abidin ◽  
Nur Amira Mamat Razali ◽  
Fauziah Abdul Aziz ◽  
...  

The main component in natural fibre is cellulose (C6H10O5)n. Cellulose from agricultural by-product is abundant, low cost, eco-friendly, biodegradable, and renewable. This research work was prepared alpha cellulose from pineapple leaf fibre (PALF), which obtained from the leaves of pineapple plant, Ananas comosus belonged to the family Bromeliaceae. The treated and untreated samples were characterized using X-ray diffraction (XRD).


2004 ◽  
Vol 831 ◽  
Author(s):  
Balaji Raghothamachar ◽  
Michael Dudley ◽  
Buguo Wang ◽  
Michael Callahan ◽  
David Bliss ◽  
...  

ABSTRACTSingle crystal GaN substrates are a more reliable, efficient and low cost alternative to sapphire and SiC substrates that are currently being used for developing nitride based devices such as LEDs, high power FETs and laser diodes. GaN growth by two techniques are investigated here. In ammonothermal growth (analogous to hydrothermal growth which is commonly used for quartz), using potassium and lithium amide as mineralizers and GaN powders and vapor grown polycrystals as nutrients, thick GaN single crystal layers have been grown on both faces of (0001) HVPE GaN seeds in nickel based autoclaves. In GaN sublimation growth, Ga is transported under a temperature gradient in an ammonia atmosphere from a GaN powder source to the sapphire substrate which has a 3–6 micron GaN epilayer deposited on it. Synchrotron white beam x-ray topography (SWBXT) was initially used to image the defect structures in the layers. High resolution x-ray diffraction experiments were also carried out and reciprocal space maps were recorded from the grown GaN layers. Characterization results will be discussed with respect to the growth conditions.


2020 ◽  
Vol 12 ◽  
Author(s):  
Md. Shoriful Islam ◽  
M. A. Sattar ◽  
M. A. Halim ◽  
Md. Asadul Hoque ◽  
Abdul Quader ◽  
...  

Background: Sand is one of the efficient sources of Silicon. We get quite easily the plethora of sand from the river side, Bangladesh. Utilization of the superfluous sand can be assisted to enhance our economy. Methods: In this work, silicon is extracted from sand by metal–thermite reduction process and the sample of sand is collected from padma river Rajshahi, Bangladesh. The process is environmentally benign and low cost. The reduction of the sand was performed with Mg powder, and purification was done by leaching out with HCl and HF. We have studied the structural properties, chemical nature and physical morphology. Results and conclusion: X-ray Diffraction (XRD) confirmed that the presence of elemental Si in the samples produced by Mg-thermite reduction process and the particle size was found 25.72±1.3 nm in an average. Surface morphology has been studied using Scanning Electron Microscopy (SEM) and the particle size seemed around 30 to 40 nm which was comparable to the obtained particle size from XRD. Fourier transform infrared spectroscopy (FTIR) showed the presence of Si-Si bonding in the investigating materials. The chemical nature of the sand has been studied by X-ray Fluorescence (XRF) analysis. Silicon content of sand was found about maximum 80%.


2015 ◽  
Vol 645-646 ◽  
pp. 32-39
Author(s):  
Zhen Guo ◽  
Lan Lu ◽  
Jing Yun Wang ◽  
Ying Jie Xing

Bi2Te3 nanowires are prepared by a low-cost and facile hydrothermal method without any surfactant. The structure and morphology of the nanowires are characterized by X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscope. The influences of experimental conditions on the products are investigated. The growth mechanism is proposed based on the experimental results. This work is promising for the synthesis of Bi2Te3 nanowires with less impurity.


2020 ◽  
Vol 860 ◽  
pp. 75-80
Author(s):  
Mochamad Zainuri ◽  
Triwikantoro ◽  
Pelangi Az Zahra

A cathode Lithium Ferro Phospate (LFP) composite material with variation doping ion Silicon (Si) with x = 0; 0,01; 0,03; 0.06 and carbon coating (LiFeSixP1-xO4/C) as lithium ion battery cathode were synthesized by a solid state reaction and wet milling methods. X-Ray Diffraction (XRD) pattern showed that the of olivine phase formed, and analysis characterization of Scanning Electron Microscopy (SEM) have shown average dimension particle of cathode in orde 1 micron. Analysis by Cyclic Voltammetry (CV) doping ion Si x = 0,03 have the best reversible electrochemical process than the other concentration, and have the highest charge and discharge capacity (78,745 mAh/g).


2015 ◽  
Vol 804 ◽  
pp. 133-136
Author(s):  
Noosara Kaewgabkam ◽  
Nittaya Jaitanong ◽  
Suparut Narksitipan

Titanium dioxide (TiO2) is the most widely used photocatalyst because of its high photocatalytic activity and reasonably low cost. Moreover, TiO2 has strong chemical stability in a large variety of environmental conditions. The combination of TiO2 with cementatious materials has been widely investigated, and the effects of the TiO2 contents (10-40% by weight) were studied in this research. The crystalline structures and chemical compositions were analyzed using x-ray diffraction (XRD) and energy dispersive x-ray spectroscopy (EDS), respectively. Moreover, its microstructure was investigated by scanning electron microscopy (SEM). It was found that the intensity of CS and CH decreased with an increase in the TiO2 powder content. This was because when adding more TiO2 powder to the composite system, more water was needed to add to the hydration reaction.


2011 ◽  
Vol 117-119 ◽  
pp. 1433-1436 ◽  
Author(s):  
Feng Hong Li ◽  
Yong Sun ◽  
San Xi Li ◽  
Shao Jun Ma

A series of acylated chitosan oligosaccharides (LCSOs) were synthesized by reacting chitosan oligosaccharide (CSO) with lauroyl chloride in methane sulfonic acid. The chemical structures of LCSOs were characterized by Fourier transform infrared. Differential scanning calorimetry (DSC) showed that LCSOs had two phase transitions during heating. Thermoplastic chitosan oligosaccharide (LCSO-4) has distinct melting temperature (Tm) at 64 °C and 110°C. X-ray diffraction (XRD) analyses indicated that the crystal structure of CSO was changed through acylation and had created new crystal domains of lauroyl side chains. New strong diffraction peaks were observed around 2θ values of 20.0°, 21.5° and 26.3° for thermoplastic acylated chitosan oligosaccharide (LCSO-4). The melting and crystallization properties of thermoplastic acylated chitosan oligosaccharide were observed by polarized optical microscope (POM).


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