scholarly journals An Insight into Chemistry and Structure of Colloidal 2D-WS2 Nanoflakes: Combined XPS and XRD Study

Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.

2021 ◽  
Vol 17 ◽  
Author(s):  
Ke Huan ◽  
Li Tang ◽  
Dongmei Deng ◽  
Huan Wang ◽  
Xiaojing Si ◽  
...  

Background: Hydrogen peroxide (H2O2) is a common reagent in the production and living, but excessive H2O2 may enhance the danger to the human body. Consequently, it is very important to develop economical, fast and accurate techniques for detecting H2O2. Methods: A simple two-step electrodeposition process was applied to synthesize Pd-Cu/Cu2O nanocomposite for non-enzymatic H2O2 sensor. Cu/Cu2O nanomaterial was firstly electrodeposited on FTO by potential oscillation technique, and then Pd nanoparticles were electrodeposited on Cu/Cu2O nanomaterial by cyclic voltammetry. The chemical structure, component, and morphology of the synthesized Pd-Cu/Cu2O nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The electrochemical properties of Pd-Cu/Cu2O nanocomposite were studied by cyclic voltammetry and amperometry. Results: Under optimal conditions, the as-fabricated sensor displayed a broad linear range (5-4000 µM) and low detection limit (1.8 µM) for the determination of H2O2. The proposed sensor showed good selectivity and reproducibility. Meanwhile, the proposed sensor has been successfully applied to detect H2O2 in milk. Conclusion: The Pd-Cu/Cu2O/FTO biosensor exhibits excellent electrochemical activity for H2O2 reduction, which has great potential application in the field of food safety.


2019 ◽  
Vol 5 (4) ◽  
pp. 61 ◽  
Author(s):  
Raja ◽  
Esquenazi ◽  
Jones ◽  
Li ◽  
Brinson ◽  
...  

In this work, as-received HiPCO single walled carbon nanotubes (SWCNTs) are incorporated in a controllable manner at various concentrations into Cu-SWCNT composites via electroless plating, by varying the related reaction times, with polyethylene glycol (PEG) used as a dispersing agent. The resultant samples were analyzed using scanning electron microscopy (SEM) for morphology assessment, energy dispersive X-ray analysis (EDX) and X-ray photoelectron spectroscopy (XPS) for elemental analysis, X-ray diffraction (XRD) for the assessment of crystal phase identification, and Raman spectroscopy for the confirmation of the presence of the incorporated SWCNTs. The Cu-SWCNT composites were found to contain carbon, catalytic iron (associated with the raw, as-received SWCNTs), oxygen, and copper; the latter was found to be inversely proportional to carbon and iron contents. The oxygen (associated with both the SWCNT defect sites and oxidized copper surfaces) remained more or less constant regardless of the proportion of SWCNTs in the composites. The Raman IG:ID ratio remains within the experimental error constant, indicating that the electroless deposition does not have a deleterious effect on the SWCNTs. At short deposition times, SEM revealed a relatively dense structure comprising a distinctive fibrous morphology, suggestive of an underlying SWCNT substrate coated with copper; however, with increasing deposition, a more porous morphology is observed. The size of the granular particles increases up until 10 min of reaction, after which time it remains unchanged.


2007 ◽  
Vol 43 (1) ◽  
pp. 21-28 ◽  
Author(s):  
C. Tang ◽  
Y. Du ◽  
H. Xu ◽  
S. Hao ◽  
L. Zhang

To ascertain whether the liquid miscibility gap exists in the Ce-Mn system, 3 key alloys are prepared by arc melting the pure elements, annealed at specified temperature for 20 minutes, quenched in ice water and then subjected to X-ray diffraction (XRD) analysis for phase identification and to scanning electron microscopy (SEM) with energy dispersive X-ray analysis for microstructure observation and composition analysis. The XRD examination indicated that terminal solutions based on Ce and Mn exist in the water-quenched alloys. No compound was detected. Microstructure observation and composition analysis indicate the nonexistence of the liquid miscibility gap. The newly assessed Ce-Mn phase diagram was presented. .


2014 ◽  
Vol 08 (02) ◽  
pp. 211-215 ◽  
Author(s):  
Yeliz Guven ◽  
Elif Bahar Tuna ◽  
Muzaffer Emin Dincol ◽  
Oya Aktoren

ABSTRACT Objective: The purpose of this study was to investigate and compare the crystalline structures of recently released MTA Plus (MTA-P), MTA Angelus (MTA-A), DiaRoot BioAggregate (BA) by X-ray diffraction (XRD) analysis. Materials and Methods: Phase analysis was carried out on powder and set forms of tested materials. The powder specimens placed into sample holders that were packed with a glass slide and the set samples prepared according to the manufacturer's instructions were placed into molds. The samples after being set for three days at 37°C and 100% humidity in an incubator were mounted onto the XRD machine and phase identification was accomplished using a search-match software program. Results: XRD findings indicated that major constituents of MTA-P were bismuth oxide, portlandite, dicalcium silicate and tricalcium silicate. The crystal structure of MTA-A were similar to those of MTA-P except for the absence of portlandite. Additionally, MTA-A had tricalcium aluminate differing from MTA-P. BA mainly differed from MTA-P and MTA-A by the radiopacifier (tantalum oxide-TO) in its composition. Conclusions: The majority of constituents of the tested materials have shown similarity except for the presence of tricalcium aluminate in MTA-A and the inclusion of TO in BA. In addition, set MTA-P showed a strong peak of portlandite.


2007 ◽  
Vol 124-126 ◽  
pp. 1229-1232 ◽  
Author(s):  
Myoung Seok Sung ◽  
Yoon Bok Lee ◽  
Yong Jin Kim ◽  
Yang Do Kim

Cadmium selenide(CdSe) nanoparticles were prepared in the aqueous solution containing isopropyl alcohol by the ultrasonic irradiation at room temperature. The cadmium chloride (CdCl2) and sodium selenosulfate (Na2SeSO3) were used as the cadmium and selenium source, respectively. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), UV-Vis absorption spectra and PL spectra were used to characterize the CdSe nanoparticles. XRD analysis revealed the formation of cubic structure CdSe. TEM images showed aggregated CdSe nanoparticles with the size of nanometer scale. Average size of CdSe nanoparticles were about 3.9, 5.0 and 5.1nm with sonication time of 6, 30 and 40 minutes, respectively. The surface emission became less intensive and shifted to red with increasing irradiation time. This paper presents the effects of ultrasonic on the formation of CdSe nanoparticles and its characteristics.


2021 ◽  
Vol 40 (2) ◽  
pp. 269-274
Author(s):  
N. Salahudeen ◽  
U. Mohammed ◽  
M.N. Yahya

Chemical, morphological characterizations and drilling mud yield point impact of Ririwai biotite have been investigated and reported in this work. Local Ririwai biotite mined in Doguwa Local Government Area of Kano State was used as a weighting agent in drilling mud formulation. Scanning Electron Microscopy (SEM) characterization, X-ray Diffraction (XRD) and Electron Dispersion X-ray (EDX) analysis of the Ririwai biotite were carried out. Water-based drilling mud was prepared using commercial bentonite according to the API 13A Standard. Effect of gradual addition of Ririwai weighting agent; 0 – 100 wt%, on the yield point of the formulated drilling mud was studied. XRD analysis showed that the dominant mineral phase in the material was biotite. Morphological analysis carried out showed that the Ririwai biotite had a sheet-like morphology while the commercial bentonite had clumpy morphology. The estimated average particle sizes were 60 and 25 μm for the Ririwai biotite and commercial bentonite, respectively. EDX analysis showed that silica-alumina ratio of the Ririwai biotite was 9.3 while that of the commercial bentonite was 1.58. The optimum yield point of the formulated drilling mud was 2.0 lb/100 ft2 corresponding to formulation having 0 – 30 wt% weighting agent composition. The specific gravity of Ririwai biotite was determined as 2.4.


Nanomaterials ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 85
Author(s):  
Patnamsetty Chidanandha Nagajyothi ◽  
Kisoo Yoo ◽  
Rajavaram Ramaraghavulu ◽  
Jaesool Shim

In this study, manganese tungstate (MW) and MW/graphene oxide (GO) composites were prepared by a facile hydrothermal synthesis at pH values of 7 and 12. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy were used for the structural, compositional, and morphological characterization of the nanoparticles (NPs). The XRD analysis revealed that the formation of monoclinic MnWO4 did not have impurities. The SEM and TEM analyses showed that the synthesized NPs were rod-shaped and well-distributed on the GO. The as-synthesized samples can be used as electrocatalysts for the urea oxidation reaction (UOR). The MW@GO-12 electrocatalyst exhibited higher current density values compared to other electrocatalysts. This study provides a new platform for synthesizing inexpensive nanocomposites as promising electrocatalysts for energy storage and conversion applications.


2019 ◽  
Vol 10 ◽  
pp. 9-21 ◽  
Author(s):  
Florian Dumitrache ◽  
Iuliana P Morjan ◽  
Elena Dutu ◽  
Ion Morjan ◽  
Claudiu Teodor Fleaca ◽  
...  

Zn/F co-doped SnO2 nanoparticles with a mean diameter of less than 15 nm and a narrow size distribution were synthesized by a one-step laser pyrolysis technique using a reactive mixture containing tetramethyltin (SnMe4) and diethylzinc (ZnEt2) vapors, diluted Ar, O2 and SF6. Their structural, morphological, optical and electrical properties are reported in this work. The X-ray diffraction (XRD) analysis shows that the nanoparticles possess a tetragonal SnO2 crystalline structure. The main diffraction patterns of stannous fluoride (SnF2) were also identified and a reduction in intensity with increasing Zn percentage was evidenced. For the elemental composition estimation, energy dispersion X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) measurements were performed. In general, both analyses showed that the Zn percentage increases with increasing ZnEt2 flow, accompanied at the same time by a decrease in the amount of F in the nanopowders when the same SF6 flow was employed. The Raman spectra of the nanoparticles show the influence of both Zn and F content and crystallite size. The fluorine presence is due to the catalytic partial decomposition of the SF6 laser energy transfer agent. In direct correlation with the increase in the Zn doping level, the bandgap of co-doped nanoparticles shifts to lower energy (from 3.55 to 2.88 eV for the highest Zn dopant concentration).


2010 ◽  
Vol 177 ◽  
pp. 92-95 ◽  
Author(s):  
Ming Yi Wang ◽  
Zong De Liu ◽  
Li Ping Zhao

This paper reports an investigation of the effect of Nb additions on the microstructure of TiC–Ni cermets, which is prepared by plasma cladding technique. The composition of the cermets cladding layer was observed by scanning electron microscope (SEM) in combination with energy dispersive spectrometer (EDS), and X-ray diffraction (XRD) analysis was carried out for phase identification. The microstructure has a trend to become finer with the increase of Nb additions, however, when the Nb addition goes to 15 wt%, the ceramic particles become much bigger and cause large amounts of cracks. Then the component variation of different parts of the ceramic particle was analyzed using the EDS, and explained the reason of the variation and why the rim structure wasn't formed.


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