scholarly journals Optimization of Parameters and Methodology for the Synthesis of LTA-Type Zeolite Using Light Coal Ash

2020 ◽  
Vol 10 (20) ◽  
pp. 7332
Author(s):  
Thiago J. T. Cruz ◽  
Mariele I. S. Melo ◽  
Sibele Pergher

The synthesis of zeolites using waste as a source of Si and Al is well known, and light coal ash has been studied to minimize the problems of waste management and mitigate environmental effects. The residue used in this work was supplied by Coal Workers Assistance Society (SATC) Criciúma–SC/Brazil, and had 24.09% Al2O3 and 54.25% SiO2 in its chemical composition. Synthesis studies using this residue with the objective of obtaining LTA zeolites were carried out by hydrothermal means, alkaline fusion, and the combination of the two methods, varying parameters such as crystallization time, Na/T ratio, OH/ratio, ultrasound exposure, gel agitation temperature, and the alkaline melting temperature of the residue. The results were characterized by X-ray diffraction (XRD) techniques and scanning electron microscopy (SEM-FEG). It was possible to obtain 70% crystalline zeolite type LTA for the first time at mild conditions with temperatures below 200 °C by alkaline fusion with smaller amounts of NaOH and short times (2 h). Thus, suitable parameters were determined for future scaling.

Materials ◽  
2021 ◽  
Vol 15 (1) ◽  
pp. 202
Author(s):  
Dumitru Doru Burduhos Nergis ◽  
Petrica Vizureanu ◽  
Andrei Victor Sandu ◽  
Diana Petronela Burduhos Nergis ◽  
Costica Bejinariu

Coal ash-based geopolymers with mine tailings addition activated with phosphate acid were synthesized for the first time at room temperature. In addition, three types of aluminosilicate sources were used as single raw materials or in a 1/1 wt. ratio to obtain five types of geopolymers activated with H3PO4. The thermal behaviour of the obtained geopolymers was studied between room temperature and 600 °C by Thermogravimetry-Differential Thermal Analysis (TG-DTA) and the phase composition after 28 days of curing at room temperature was analysed by X-ray diffraction (XRD). During heating, the acid-activated geopolymers exhibited similar behaviour to alkali-activated geopolymers. All of the samples showed endothermic peaks up to 300 °C due to water evaporation, while the samples with mine tailings showed two significant exothermic peaks above 400 °C due to oxidation reactions. The phase analysis confirmed the dissolution of the aluminosilicate sources in the presence of H3PO4 by significant changes in the XRD patterns of the raw materials and by the broadening of the peaks because of typically amorphous silicophosphate (Si–P), aluminophosphate (Al–P) or silico-alumino-phosphate (Si–Al–P) formation. The phases resulted from geopolymerisation are berlinite (AlPO4), brushite (CaHPO4∙2H2O), anhydrite (CaSO4) or ettringite as AFt and AFm phases.


2020 ◽  
Vol 8 (1) ◽  
pp. 19-22
Author(s):  
Kanaan R. Ahmed

In this work, it is shown that based on powder zeolite type Y, mono metallic and bimetallic catalysts have been developed that are promising for petroleum chemistry processes. The method is based on the preparing hydrogen form of Y zeolite by ion exchange with a solution of ammonium nitrate at a starting concentration of 70 g.l-1 and nickel nitrate solution which provides Ni cations. Then after preparation of bimetallic catalysts by impregnating second metal by incipient wetness. All samples and catalysts were characterized using X-ray diffraction (XRD) analysis techniques, adsorption methods, and elemental analysis. The research results showed that in order to reach the degree of exchange of Na+ for H+ cations  no less than 0.73, it is necessary to carry out four exchanges of Na+ by NH4+ and three intermediate thermal treatments at 540 °C for 3 to 4 hours in air atmosphere.


Author(s):  
G. A. Bertero ◽  
W.H. Hofmeister ◽  
N.D. Evans ◽  
J.E. Wittig ◽  
R.J. Bayuzick

Rapid solidification of Ni-Nb alloys promotes the formation of amorphous structure. Preliminary results indicate promising elastic properties and high fracture strength for the metallic glass. Knowledge of the thermal stability of the amorphus alloy and the changes in properties with temperature is therefore of prime importance. In this work rapidly solidified Ni-Nb alloys were analyzed with transmission electron microscopy (TEM) during in-situ heating experiments and after isothermal annealing of bulk samples. Differential thermal analysis (DTA), scanning electron microscopy (SEM) and x-ray diffraction (XRD) techniques were also used to characterize both the solidification and devitrification sequences.Samples of Ni-44 at.% Nb were electromagnetically levitated, melted, and rapidly solidified by splatquenching between two copper chill plates. The resulting samples were 100 to 200 μm thick discs of 2 to 3 cm diameter. TEM specimens were either ion-milled or alternatively electropolished in a methanol-10% sulphuric acid solution at 20 V and −40°C.


Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Carlos Alberto Ríos-Reyes ◽  
German Alfonso Reyes-Mendoza ◽  
José Antonio Henao-Martínez ◽  
Craig Williams ◽  
Alan Dyer

This study reports for the first time the geologic occurrence of natural zeolite A and associated minerals in mudstones from the Cretaceous Paja Formation in the urban area of the municipality of Vélez (Santander), Colombia. These rocks are mainly composed of quartz, muscovite, pyrophyllite, kaolinite and chlorite group minerals, framboidal and cubic pyrite, as well as marcasite, with minor feldspar, sulphates, and phosphates. Total organic carbon (TOC), total sulfur (TS), and millimeter fragments of algae are high, whereas few centimeters and not biodiverse small ammonite fossils, and other allochemical components are subordinated. Na–A zeolite and associated mineral phases as sodalite occur just beside the interparticle micropores (honeycomb from framboidal, cube molds, and amorphous cavities). It is facilitated by petrophysical properties alterations, due to processes of high diagenesis, temperatures up to 80–100 °C, with weathering contributions, which increase the porosity and permeability, as well as the transmissivity (fluid flow), allowing the geochemistry remobilization and/or recrystallization of pre-existing silica, muscovite, kaolinite minerals group, salts, carbonates, oxides and peroxides. X-ray diffraction analyses reveal the mineral composition of the mudstones and scanning electron micrographs show the typical cubic morphology of Na–A zeolite of approximately 0.45 mμ in particle size. Our data show that the sequence of the transformation of phases is: Poorly crystalline aluminosilicate → sodalite → Na–A zeolite. A literature review shows that this is an unusual example of the occurrence of natural zeolites in sedimentary marine rocks recognized around the world.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2623
Author(s):  
Monika Wójcik-Bania ◽  
Jakub Matusik

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.


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


Surfaces ◽  
2021 ◽  
Vol 4 (2) ◽  
pp. 106-114
Author(s):  
Yannick Hermans ◽  
Faraz Mehmood ◽  
Kerstin Lakus-Wollny ◽  
Jan P. Hofmann ◽  
Thomas Mayer ◽  
...  

Thin films of ZnWO4, a promising photocatalytic and scintillator material, were deposited for the first time using a reactive dual magnetron sputtering procedure. A ZnO target was operated using an RF signal, and a W target was operated using a DC signal. The power on the ZnO target was changed so that it would match the sputtering rate of the W target operated at 25 W. The effects of the process parameters were characterized using optical spectroscopy, X-ray diffraction, and scanning electron microscopy, including energy dispersive X-ray spectroscopy as well as X-ray photoelectron spectroscopy. It was found that stoichiometric microcrystalline ZnWO4 thin films could be obtained, by operating the ZnO target during the sputtering procedure at a power of 55 W and by post-annealing the resulting thin films for at least 10 h at 600 °C. As FTO coated glass substrates were used, annealing led as well to the incorporation of Na, resulting in n+ doped ZnWO4 thin films.


Energies ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1230
Author(s):  
Jessica Manzi ◽  
Annalisa Paolone ◽  
Oriele Palumbo ◽  
Domenico Corona ◽  
Arianna Massaro ◽  
...  

In this manuscript, we report a detailed physico-chemical comparison between the α- and β-polymorphs of the NaMnO2 compound, a promising material for application in positive electrodes for secondary aprotic sodium batteries. In particular, the structure and vibrational properties, as well as electrochemical performance in sodium batteries, are compared to highlight differences and similarities. We exploit both laboratory techniques (Raman spectroscopy, electrochemical methods) and synchrotron radiation experiments (Fast-Fourier Transform Infrared spectroscopy, and X-ray diffraction). Notably the vibrational spectra of these phases are here reported for the first time in the literature as well as the detailed structural analysis from diffraction data. DFT+U calculations predict both phases to have similar electronic features, with structural parameters consistent with the experimental counterparts. The experimental evidence of antisite defects in the beta-phase between sodium and manganese ions is noticeable. Both polymorphs have been also tested in aprotic batteries by comparing the impact of different liquid electrolytes on the ability to de-intercalated/intercalate sodium ions. Overall, the monoclinic α-NaMnO2 shows larger reversible capacity exceeding 175 mAhg−1 at 10 mAg−1.


2011 ◽  
Vol 170 ◽  
pp. 165-169 ◽  
Author(s):  
Tahir Ali ◽  
Ernst Bauer ◽  
Gerfried Hilscher ◽  
Herwig Michor

We report on structural and superconducting properties of La3-xRxNi2B2N3- where La is substituted by the magnetic rare-earth elements Ce, Pr, Nd. The compounds Pr3Ni2B2N3- and Nd3Ni2B2N3- are characterized for the first time. Powder X-ray diffraction confirmed all samples R3Ni2B2N3- with R = La, Ce, Pr, Nd and their solid solutions to crystallize in the body centered tetragonal La3Ni2B2N3 structure type. Superconducting and magnetic properties of La3-xRxNi2B2N3- were studied by resistivity, specific heat and susceptibility measurements. While La3Ni2B2N3- has a superconducting transition temperature Tc ~ 14 K, substitution of La by Ce, Pr, and Nd leads to magnetic pair breaking and, thus, to a gradual suppression of superconductivity. Pr3Ni2B2N3- exibits no long range magnetic order down to 2 K, Nd3Ni2B2N3- shows ferrimagnetic ordering below TC =17 K and a spin reorientation transition to a nearly antiferromagnetic state at 10 K.


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