scholarly journals Mössbauer and X-ray Studies of Phase Composition of Fly Ashes Formed after Combustion of Ekibastuz Coal (Kazakhstan)

Metals ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 929
Author(s):  
Adilkhan Shokanov ◽  
Mikhail Vereshchak ◽  
Irina Manakova

Mössbauer spectroscopy and X-ray diffraction have been used to study samples of fly ashes formed after combustion of coal from the Ekibastuz basin at the thermal power plants TPP-2 and TPP-3 in Almaty (Kazakhstan). It has been established that the fractions of fly ashes contain iron in the form of magnetite Fe3O4 and hematite α-Fe2O3. The mixed valence of iron Fe3+ ↔ Fe2+ in the octahedral sublattice of magnetite is destroyed by isostructural substitution impurities. Maghemite γ-Fe2O3 is additionally present in the fly ash of TPP-3 as a product of magnetite slow oxidation. It was shown that at T ≥ 1400 °C the proportion of magnetite in fly ashes increases due to decomposition of hematite, maghemite, hercynite and the drop of iron content in mullite. It was concluded that the amount of iron in magnetite is a temperature indicator of fly ashes formation. The parameters of hyperfine interactions have been determined in the iron-containing minerals of fly ashes. It was identified that formation of the fly ashes structure occurs in oxidizing atmosphere, since no traces were revealed of reducing environment effect on the phase composition.

2012 ◽  
Vol 452-453 ◽  
pp. 77-80 ◽  
Author(s):  
Shou Jun Wu ◽  
Gutmanas Elazar

In order to improve oxidation/erosion resistance of the T/P 24 steel components used in advanced power plants, chrome carbide coatings were prepared by PIRAC (Powder Immersion Reaction Assisted Coating) on T/P24 at 700-1000°C. Microstructure and phase composition of the obtained surface layers were characterized employing X-ray diffraction and scanning electron microscopy with chemical analysis (SEM/EDS). Results showed that homogenous smooth chrome carbide coatings can be formed on the substrate. Phase composition of the prepared coatings are differs with PIRAC temperatures. Prepared at lower temperatures or short times treatment, Cr23C6, Cr7C3 and Cr3C2 can be detected in the coatings. While, at higher temperatures or longer treatment times, Cr23C6 is subtotal phase of the produced coating. Moreover, the lower the PIRAC temperature is, the more of Cr7C3 and Cr3C2 are. Thermodynamics calculation based on Gibbs free energy is applied to explain phase composition difference of the coatings.


Crystals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1064
Author(s):  
Denitza Zgureva ◽  
Valeria Stoyanova ◽  
Annie Shoumkova ◽  
Silviya Boycheva ◽  
Georgi Avdeev

Worldwide disposal of multi-tonnage solid waste from coal-burning thermal power plants (TPPs) creates serious environmental and economic problems, which necessitate the recovery of industrial waste in large quantities and at commercial prices. Fly ashes (FAs) and slag from seven Bulgarian TPPs have been successfully converted into valuable zeolite-like composites with various applications, including as adsorbents for capturing CO2 from gases and for removal of contaminants from water. The starting materials generated from different types of coal are characterized by a wide range of SiO2/Al2O3 ratio, heterogeneous structure and a complex chemical composition. The applied synthesis procedure resembles the formation of natural zeolites, as the raw FAs undergo long-term self-crystallization in an alkaline aqueous solution at ambient temperature. The phase and chemical composition, morphology and N2 adsorption of the final zeolite products were studied by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), X-Ray Diffraction (XRD) and Brunauer–Emmett–Teller (BET) analyses. The growth of faujasite (FAU) crystals as the main zeolite phase was established in all samples after 7 and 14 months of alkaline treatment. Phillipsite (PHI) crystals were also observed in several samples as an accompanying phase. The final products possess specific surface area over 400 m2/g. The relationships between the surface properties of the investigated samples and the characteristics of the raw FAs were discussed. All of the obtained zeolite-like composites were able to remove the highly toxic dye (malachite green, MG) from water solutions with efficiency over 96%. The experimental data were fitted with high correlation to the second-order kinetics.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


2019 ◽  
Vol 484 (1) ◽  
pp. 41-43
Author(s):  
E. A. Malinina ◽  
V. K. Skachkova ◽  
I. V. Kozerozhets ◽  
V. V. Avdeeva ◽  
L. V. Goeva ◽  
...  

The method of nanoscaled sodium dodecahydro-closo-dodecaborate Na2[B12H12] synthesis is presented. The composite is heated to 200°C to yield the desired product, forming with the introduction of triethyl- ammonium salt [Et3NH]2[B12H12] into the silicate matrix of a sodium liquid glass. The morphology and phase composition of the synthesized sample are studied through SEM and X-ray diffraction methods, in comparison to those of a standard salt sample Na2[B12H12]. Based on the obtained data, the sample under study is an amorphous composite, on the surface of which nanoscale crystals of Na2[B12H12] form.


Author(s):  
Tianlei Ma ◽  
Marek Nikiel ◽  
Andrew G. Thomas ◽  
Mohamed Missous ◽  
David J. Lewis

AbstractIn this report, we prepared transparent and conducting undoped and molybdenum-doped tin oxide (Mo–SnO2) thin films by aerosol-assisted chemical vapour deposition (AACVD). The relationship between the precursor concentration in the feed and in the resulting films was studied by energy-dispersive X-ray spectroscopy, suggesting that the efficiency of doping is quantitative and that this method could potentially impart exquisite control over dopant levels. All SnO2 films were in tetragonal structure as confirmed by powder X-ray diffraction measurements. X-ray photoelectron spectroscopy characterisation indicated for the first time that Mo ions were in mixed valence states of Mo(VI) and Mo(V) on the surface. Incorporation of Mo6+ resulted in the lowest resistivity of $$7.3 \times 10^{{ - 3}} \Omega \,{\text{cm}}$$ 7.3 × 10 - 3 Ω cm , compared to pure SnO2 films with resistivities of $$4.3\left( 0 \right) \times 10^{{ - 2}} \Omega \,{\text{cm}}$$ 4.3 0 × 10 - 2 Ω cm . Meanwhile, a high transmittance of 83% in the visible light range was also acquired. This work presents a comprehensive investigation into impact of Mo doping on SnO2 films synthesised by AACVD for the first time and establishes the potential for scalable deposition of SnO2:Mo thin films in TCO manufacturing. Graphical abstract


Materials ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1267
Author(s):  
David Längauer ◽  
Vladimír Čablík ◽  
Slavomír Hredzák ◽  
Anton Zubrik ◽  
Marek Matik ◽  
...  

Large amounts of coal combustion products (as solid products of thermal power plants) with different chemical and physical properties cause serious environmental problems. Even though coal fly ash is a coal combustion product, it has a wide range of applications (e.g., in construction, metallurgy, chemical production, reclamation etc.). One of its potential uses is in zeolitization to obtain a higher added value of the product. The aim of this paper is to produce a material with sufficient textural properties used, for example, for environmental purposes (an adsorbent) and/or storage material. In practice, the coal fly ash (No. 1 and No. 2) from Czech power plants was firstly characterized in detail (X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), particle size measurement, and textural analysis), and then it was hydrothermally treated to synthetize zeolites. Different concentrations of NaOH, LiCl, Al2O3, and aqueous glass; different temperature effects (90–120 °C); and different process lengths (6–48 h) were studied. Furthermore, most of the experiments were supplemented with a crystallization phase that was run for 16 h at 50 °C. After qualitative product analysis (SEM-EDX, XRD, and textural analytics), quantitative XRD evaluation with an internal standard was used for zeolitization process evaluation. Sodalite (SOD), phillipsite (PHI), chabazite (CHA), faujasite-Na (FAU-Na), and faujasite-Ca (FAU-Ca) were obtained as the zeolite phases. The content of these zeolite phases ranged from 2.09 to 43.79%. The best conditions for the zeolite phase formation were as follows: 4 M NaOH, 4 mL 10% LiCl, liquid/solid ratio of 30:1, silica/alumina ratio change from 2:1 to 1:1, temperature of 120 °C, process time of 24 h, and a crystallization phase for 16 h at 50 °C.


2004 ◽  
Vol 37 (6) ◽  
pp. 967-976 ◽  
Author(s):  
Andrew C. Jupe ◽  
Stuart R. Stock ◽  
Peter L. Lee ◽  
Nikhila N. Naik ◽  
Kimberly E. Kurtis ◽  
...  

Spatially resolved energy dispersive X-ray diffraction, using high-energy synchrotron radiation (∼35–80 keV), was used nondestructively to obtain phase composition profiles along the radii of cylindrical cement paste samples to characterize the progress of the chemical changes associated with sulfate attack on the cement. Phase distributions were acquired to depths of ∼4 mm below the specimen surface with sufficient spatial resolution to discern features less than 200 µm thick. The experimental and data analysis methods employed to obtain quantitative composition profiles are described. The spatial resolution that could be achieved is illustrated using data obtained from copper cylinders with a thin zinc coating. The measurements demonstrate that this approach is useful for nondestructively visualizing the sometimes complex transformations that take place during sulfate attack on cement-based materials. These transformations can be spatially related to microstructure as seen by computed microtomography.


2013 ◽  
Vol 710 ◽  
pp. 170-173
Author(s):  
Lian Ping Chen ◽  
Yuan Hong Gao

It is hardly possible to obtain rare earth doped CaWO4thin films directly through electrochemical techniques. A two-step method has been proposed to synthesize CaWO4:(Eu3+,Tb3+) thin films at room temperature. X-ray diffraction, energy dispersive X-ray analysis, spectrophotometer were used to characterize their phase, composition and luminescent properties. Results reveal that (Eu3+,Tb3+)-doped CaWO4films have a tetragonal phase. When the ratio of n (Eu)/n (Tb) in the solution is up to 3:1, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Tb element; on the contrary, when the ratio in the solution is lower than 1:4, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Eu element. Under the excitation of 242 nm, sharp emission peaks at 612, 543, 489 and 589 nm have been observed for CaWO4:(Eu3+,Tb3+) thin films.


2021 ◽  
Author(s):  
Isam M. Arafa ◽  
Mazin Y. Shatnawi ◽  
Yousef N. Obeidallah ◽  
Ahmed K. Hijazi ◽  
Yaser A . Yousef

Abstract Four transition metal borohydrides (MTBHs, MT = Ni, Fe, Co, and Cu) were prepared by sonicating a mixture of the desired MT salt with excess NaBH4 in a nonaqueous DMF/CH3OH media. The process afforded bimetallic (Ni-BH4), trimetallic (Fe-BH4, Co-BH4), and mixed-valence (Cu-H, Cu-BH4) amorphous, ferromagnetic nanoparticles as identified by thermal, ATR-IR, X-Ray diffraction, and magnetic susceptibility techniques. The electrical conductivity (σ) of cold-pressed discs of these MTBHs shows a nonlinear increase while their thermal conductivity (κ) decreases in the temperature range of 303 ≤ T ≤ 373 K. The thermal energy transport occurs through phonon lattice dynamics rather than electronic. The σ/κ ratio shows a nonlinear steep increase from 9.4 to 270 KV-2 in Ni-BH4, while a moderate-weak increase is observed for Fe-BH4, Co-BH4, and Cu-BH4. Accordingly, the corresponding thermoelectric (TE) parameters S, PF, ZT, and η were evaluated. All TE data shows that the bimetallic Ni-BH4 (S, 80 μVK-1; PF, 259 μWm-1K-2; ZT 0.64; η, 2.56%) is a better TE semiconductor than the other three MT-BHs investigated in this study. Our findings show that Ni-BH4 is a promising candidate to exploit low-temperature waste heat from body heat, sunshine, and small domestic devices for small-scale TE applications.


2014 ◽  
Vol 70 (a1) ◽  
pp. C901-C901
Author(s):  
Solveig Madsen ◽  
Jacob Overgaard ◽  
Bo Iversen

Intramolecular electron transfer (ET) in mixed valence (MV) oxo-centered [FeiiFeiii2O(carboxylate)6(ligand)3]·solvent complexes is highly dependent on temperature, on the nature of the ligands, and on the presence of crystal solvent molecules [1]. Whereas the effects of temperature, crystal solvent, and ligand variation on the details of the ET have been explored thoroughly, the effect of pressure is less well described [2]. The effect of pressure on the ET in MV Fe3O(cyanoacetate)6(water)3has been investigated with single crystal X-ray diffraction and Mössbauer spectroscopy. Previous multi-temperature studies have shown that at room temperature the ET between the three Fe sites is fast and the observed structure of the Fe3core is a perfectly equilateral triangle [3]. Cooling the complex below 130 K induces a phase transition as the ET slows down. Below 120 K the Fe3core is distorted due to the localization of the itinerant electron on one of the three Fe sites in the triangle (the complex is then in the valence trapped state). The valence trapping is complete within a temperature interval of just 10 K. The abruptness of the transition has been attributed to the extended hydrogen bond network involving water ligands and cyano groups, promoting intermolecular cooperative effects. The high-pressure X-ray diffraction data show that there is a 900flip of half the cyano groups at 3.5 GPa, which dramatically changes the hydrogen bond network. At a slightly higher pressure, a phase transition is found to occur. The five single crystals investigated all broke into minor fragments at the transition; however triclinic unit cells, similar to the low temperature unit cell, could be indexed from selected spots. Additional evidence that the complex is valence trapped comes from high pressure Mössbauer spectra measured above the phase transition (4 GPa). The relationship between valence trapping and the structural changes will in this work be highlighted using void space and Hirshfeld surface analysis.


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