scholarly journals Characterization of size and morphological composition of ablated nanoparticles of cerium dioxide after ultrasonic dispersion and centrifugation in aqueous solution

2021 ◽  
Vol 2064 (1) ◽  
pp. 012083
Author(s):  
V A Mamontov ◽  
A Yu Ryzhenkova ◽  
M A Pugachevskii

Abstract The paper investigates the size and morphological composition of ablated cerium dioxide nanoparticles after ultrasonic dispersion at centrifugation speeds from 800 to 13400 rpm. A nanodispersed solution of cerium dioxide was deposited onto silicon substrates by the drop method. To characterize the size and morphological composition of cerium dioxide nanoparticles, methods of scanning electron and atomic microscopy were used, and X-ray phase analysis was performed. It was found that ablated cerium dioxide particles in an aqueous solution agglomerated and without centrifugation their average size was 162 nm, after centrifugation their average size varied from 86 nm to 142.5 nm. X-ray phase analysis showed that with an increase in the centrifuge speed, the size of the coherent scattering region decreases, which affects the effectiveness of antioxidant properties, for example, in the Fenton reaction.

Author(s):  
V. V. Polyakov ◽  
A. V. Babin ◽  
V. A. Lebedev

The purpose of this study is to obtain highly dispersed powder suitable for spheroidization for further application in additive technologies. Volumetric reduction of the FeCl2–CaCl2melt by calcium dissolved in CaCl2produced fine iron powder. The process consisted of three stages: preparation of melts containing FeCl2and Ca, their mixing and high-temperature aging at 800 °C for 1 hour. At the end of the process the frozen melt was divided into upper and bottom parts. The product from the upper part had a specific surface area of 7,60 m2/g, and for the lower part it was 5,38 m2/g, Average particle size was 157 μm for the former and 124 μm for the latter. After ultrasonic dispersion, it was reduced to 26 μm and 71 μm, respectively. Quantitative X-ray phase analysis showed that the main phase of powder is metallic iron (more than 97 wt.%). Therefore, research originality is the use of volumetric, intensive reduction of iron from chloride melts by calcium dissolved in its chloride. The uniqueness of the study consists in the product obtained, i.e. the main part of reduced iron is in the melt volume as linear aggregates 40 to 600 μm in length, 10 to 50 μm in diameter that are easily broken by ultrasonic dispersion into individual crystals with an average size of 26 μm. The results of the study demonstrated the feasibility of calcium-thermal production of fine iron powder.


2016 ◽  
Vol 49 (1) ◽  
pp. 188-194 ◽  
Author(s):  
Mina Choi ◽  
Bahaa Ghammraoui ◽  
Andreu Badal ◽  
Aldo Badano

Small-angle X-ray scattering (SAXS) has recently been proposed as a novel noninvasivein vivomolecular imaging technique to characterize molecular interactions deep within the body using high-contrast probes. This article describes a detailed Monte Carlo X-ray transport simulation technique that utilizes user-provided cross sections to describe X-ray interaction in virtual samples and explore SAXS instrument design choices. The accuracy of the simulation code is validated with sample material cross sections derived from analytical models and empirical measurements of a homogeneous spherical gold nanoparticle (GNP) monomer, a dimer and heterogeneous mixtures of the two in aqueous solution. Analytical and measured scattering profiles from these samples were converted to cross sections using an absolute water standard. Our Monte Carlo estimates of the fraction of dimers from analytically derived and empirically derived cross sections are strongly correlated, with less than 1.5 and 16% error, respectively, to the expected concentration of monomer and dimer species. In addition, a variety of monoenergetic X-ray beams were simulated to investigate coherent scatteringversusradiation dose for a range of sample sizes. For GNP spheres in aqueous solution, the energy range that produces the most coherent scattering at the detector per deposited energy was between 31 and 49 keV for a sample thickness of 1 mm to 10 cm. The method described here for the detailed simulation of SAXS using measured and modeled cross sections will enable instrumentation optimization forin vivomolecular imaging applications.


2022 ◽  
pp. 1-6
Author(s):  
Hui Li ◽  
Meng He ◽  
Ze Zhang

Quantitative phase analysis is one of the major applications of X-ray powder diffraction. The essential principle of quantitative phase analysis is that the diffraction intensity of a component phase in a mixture is proportional to its abundance. Nevertheless, the diffraction intensities of the component phases cannot be compared with each other directly since the coherent scattering power per unit cell (or chemical formula) of each component phase is usually different. The coherent scattering power per unit cell of a crystal is well represented by the sum of the squared structure factors, which cannot be calculated directly when the crystal structure data is unavailable. Presented here is a way to approximate the coherent scattering power per unit cell based solely on the unit cell parameters and the chemical contents. This approximation is useful when the atomic coordinates for one or more of the phases in a sample are unavailable. An assessment of the accuracy of the approximation is presented. This assessment indicates that the approximation will likely be within 10% when X-ray powder diffraction data is collected over a sufficient portion of the measurable pattern.


2012 ◽  
Vol 164 ◽  
pp. 132-136
Author(s):  
Zhi Xiang Liu ◽  
Zhe Sheng Qiu ◽  
Ji Kang Yan ◽  
Guo You Gan ◽  
Rui Jiao Jia ◽  
...  

In this paper, the preparation and antioxidant properties of SnO2coating of steel claw of prebaked carbon used as electrolytic aluminium anode was investigated. A denser SnO2coating on steel claw was prepared by high temperature glaze method . Phase Analysis , microstructure and chemical composition of the steel claw antioxidant coating were by Japan Rigaku D/Max2200 type X-ray diffraction, the Philip XL30 ESEM and EDS. the Oxidation resistance experiments results showed that the better anti-oxidation coating has a optimal thickness size of about 0.4mm.


2015 ◽  
Vol 1085 ◽  
pp. 12-16
Author(s):  
Rustam Hairullin ◽  
Svetlana Dorovskikh

In this work the effect of substrate and vaporization temperatures on the structural parameters (sizes of coherent scattering region, values of strain), phase and chemical composition, surface morphology of Co films is revealed. Co films were deposited on Si (100) substrates by Metal-organic chemical vapor deposition using the diiminate complex Co (N’acN’ac)2 as a precursor. The sizes of coherent scattering region, values of strain and phase composition of Co films were determined by the X-ray diffraction analysis. The chemical composition was identified by the Energy-dispersive X-ray spectroscopy. The surface morphology of Co films was investigated by scanning electron microscope. It is found that the variation of deposition conditions allows us widely to change structural parameters and chemical composition of Co films.


2020 ◽  
Vol 21 (2) ◽  
pp. 219-226
Author(s):  
B. K. Ostafiychuk ◽  
H. M. Kolkovska ◽  
I. P. Yaremiy ◽  
B. I. Rachiy ◽  
P. I. Kolkovskyi ◽  
...  

In this work, the perovskite LaMnO3 material has been prepared based on the sol-gel process of synthesis with the participation of combustion. According to the X-ray phase analysis, it was determined that the obtained material consists of LaMnO3 one phase (space group Pm-3m). Nevertheless, it has been determined that the average size of the coherent scattering region of the obtained material is about 24 nm. Moreover, the average particle size is 40-60 nm in case the approximation that the particles are spherical shape. Thus, it has been determined that the specific surface area of the material is 42.1 m2/g. The electrochemical investigations have been performed using nanosized LaMnO3 powder as a cathode material for electrochemical capacitors. The LaMnO3 material under research showed a specific capacity of 40 F/g at a discharge of up to 1V.


2015 ◽  
Vol 16 (2) ◽  
pp. 351-354
Author(s):  
V.S. Bushkova ◽  
I.P. Yaremiy ◽  
R.V. Ilnitsky ◽  
R.P. Lisovskiy ◽  
M.L. Mokhnatskyi

The aim of this work was to create and study of ferrite nickel-cobalt powders, using sol-gel technology with participation of auto-combustion. After completing the process autocombustion was obtained only one phase, which corresponded to  the cubic structure of spinel space group Fd3m. It was found that the average size of coherent scattering regions not exceeding 62 nm. The dependences of the lattice parameter, X-ray density and specific surface area of the ferrite powders from nickel content were found. It was shown that at substitution of cations cobalt on cations nickel latest give preference only B positions, thus displacing part of in the A positions.


2021 ◽  
Author(s):  
Vil Dayanovich Sitdikov ◽  
Artyom Anatolyevich Nikolaev ◽  
Ekaterina Alekseevna Kolbosenko ◽  
Grigoriy Vladimirovich Ivanov ◽  
Artyom Konstantinovich Makatrov ◽  
...  

Abstract The article presents the results of identification and quantitative analysis of the phase composition, fine structure parameters of minerals in carbonate and terrigenous rocks by the use of modern X-ray diffraction (XRD) analysis. To make the XRD analysis, we optimized the modes of x-ray pattern shooting by changing the radius of the goniometer, the system of primary and secondary slits, Soller slits, and the system of detecting the low-content minerals. In processing the obtained x-ray patterns, we considered the size and defects of the crystal grains, the crystallographic mode of arrangements, atomic population of the crystal lattice, the Debye-Waller factor and the instrumental line broadening by the use of the Caliotti function for LaB6. So we determined the type and content of minerals, estimated the period of the crystal lattice, the size of the coherent scattering domains and micro-distortion crystal lattice of the mineral. We compared the obtained data on the presence and quantitative content of minerals with the data of X-ray fluorescence (XRF) analysis and scanning electron microscopy (SEM). Based on the obtained data, reference intensity ratio (RIR) coefficients were selected for a number of minerals typically contained in core materials for quantitative phase analysis by the use of the corundum number method.


Author(s):  
E. V. Yakushko ◽  
L. V. Kozhitov ◽  
D. G. Muratov ◽  
D. Yu. Karpenkov ◽  
A. V. Popkova

The NiCo/C metal-carbon nanocomposites based on the NiCl2/CoCl2/Polyacrylonitrile (PAN) precursors were synthesized using IR heating. The results of studies of NiCo/C nanocomposites by X-ray phase analysis, transmission electron microscopy, and vibration magnetometry showed the dependence of the structure and properties of NiCo/C nanocomposites on the synthesis temperature, concentration, and metal ratio in the precursor. According to the results of the X-ray phase analysis, it was found that during the IR pyrolysis of the precursor, NiCo metal nanoparticles are stabilized in the carbon matrix, an increase in the synthesis temperature from 350 to 800 °C leads to an increase in the average size of nio nanoparticles from 10 to 80 nm, it is established that the formation of the alloy occurs due to the gradual dissolution of cobalt in nickel with the simultaneous transition of cobalt from the hcp modification to FCC. The structure of nanocomposites was shown by transmission electron microscopy of samples synthesized at 600 °C. It was found that with an increase in the metal concentration in the precursor from 10 to 40 wt.%, the average size of NiCo nanoparticles increases and the concentration of nanoparticles in the carbon matrix increases. The study of the magnetic properties of nanocomposites showed that with an increase in the content of metals in the precursor from 10 to 40 wt.%, an almost linear increase in the saturation magnetization from 5.94 to 25.7 A · m2/kg is observed. A change in the ratio of metals from Ni : Co = 4 : 1 to Ni : Co = 1 : 4 causes an increase in magnetization from 11.46 to 23.3 A · m2/kg.


2019 ◽  
Vol 20 (4) ◽  
pp. 360-366
Author(s):  
Yu.V. Yavorskyi ◽  
Ya.V. Zaulychnyy ◽  
М.V. Karpets ◽  
А.B. Hrubiak ◽  
V.V. Moklyak ◽  
...  

Using the method of X-ray diffraction, the effect of shock-vibration treatment on the structural parameters and phase composition of mixtures of silicon dioxide and alpha iron oxide was studied. From these results, has been found that the shock-vibration treatment of oxides mixture leads to an increase in the coherent scattering region of crystalline α-Fe2O3. We obtained SEM images of composites before and after treatment. From the SEM images it is seen that the processing is accompanied by fragmentation of the aggregates, uniform placement of the nanoparticles between each other and the formation of new denser agglomerates. Electron-microscopic study of mixtures using TEM was performed, which showed that the treatment leads to a lay-up of particles each other with the formation of interatomic interaction between them, which is consistent with the results of ultra-soft X-ray emission spectroscopy. The electrochemical properties of LPS, with electrodes based on mixtures before and after treatment, in galvanostatic mode were investigated. It is found that the charge capacity of the LPS with the electrode based on the mixture with the maximum concentration of α-Fe2O3 after treatment is reduced by half. 


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