Search results for: x-ray diffraction analysis

Authors: M. Mana, M. S. Ouali, L. C. de Menorval

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A spent bleaching earth from an edible oil refinery has been treated by impregnation with a normal sodium hydroxide solution followed by mild thermal treatment (100°C). The obtained material (TSBE) was washed, dried and characterized by X-ray diffraction, FTIR, SEM, BET, and thermal analysis. The clay structure was not apparently affected by the treatment and the impregnated organic matter was quantitatively removed. We have investigated the comparative sorption of safranine and methylene blue on this material, the spent bleaching earth (SBE) and the virgin bleaching earth (VBE). The kinetic results fit the pseudo second order kinetic model and the Weber & Morris, intra-particle diffusion model. The pH had no effect on the sorption efficiency. The sorption isotherms followed the Langmuir model for various sorbent concentrations with good values of determination coefficient. A linear relationship was found between the calculated maximum removal capacity and the solid/solution ratio. A comparison between the results obtained with this material and those of the literature highlighted the low cost and the good removal capacity of the treated spent bleaching earth.

Keywords: basic dyes, isotherms, sorption, spent bleaching earth

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Authors: Tsung-Yen Tsai, Naveen Bunekar, Ming Hsuan Chang, Wen-Kuang Wang, Satoshi Onda

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The structure-property relationship and initiator effect on bulk polymerized poly(methyl methacrylate) (PMMA)–oragnomodified layered silicate nanocomposites was investigated. In this study, we used 2, 2'-azobis (4-methoxy-2,4-dimethyl valeronitrile and benzoyl peroxide initiators for bulk polymerization. The bulk polymerized nanocomposites’ morphology was investigated by X-ray diffraction and transmission electron microscopy. The type of initiator strongly influences the physiochemical properties of the polymer nanocomposite. The thermal degradation of PMMA in the presence of nanofiller was studied. 5 wt% weight loss temperature (T5d) increased as compared to pure PMMA. The peak degradation temperature increased for the nanocomposites. Differential scanning calorimetry and dynamic mechanical analysis were performed to investigate the glass transition temperature and the nature of the constrained region as the reinforcement mechanism respectively. Furthermore, the optical properties such as UV-Vis and Total Luminous Transmission of nanocomposites are examined.

Keywords: initiator, bulk polymerization, layered silicates, methyl methacrylate

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Authors: Justyna Chrzanowska, Jacek Hoffman, Dariusz Garbiec, Łukasz Kurpaska, Piotr Denis, Tomasz Moscicki, Zygmunt Szymanski

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Tungsten and boron compounds belong to the group of superhard materials and its hardness could exceed 40 GPa. In this study, the properties of the tungsten boride (WB) layers deposited in magnetron sputtering process are investigated. The sputtering process occurred from specially prepared targets that were composed of boron and tungsten mixed in molar ratio of 2.5 or 4.5 and sintered in spark plasma sintering process. WB layers were deposited on silicon (100) and stainless steel 304 substrates at room temperature (RT) or in 570 °C. Layers deposited in RT and in elevated temperature varied considerably. Layers deposited in RT are amorphous and have low adhesion. In contrast, the layers deposited in 570 °C are crystalline and have good adhesion. All deposited layers have a hardness about 40 GPa. Moreover, the friction coefficient of crystalline layers is 0.22 and wear rate is about 0.67•10-6 mm3N-1m-1. After material characterization the WB layers were annealed in argon atmosphere in 1000 °C for 1 hour. On the basis of X-Ray Diffraction analysis, it has been noted that the crystalline layers are thermally stable and do not change their phase composition, whereas the amorphous layers change their phase composition. Moreover, after annealing, on the surface of WB layers some cracks were observed. It is probably connected with the differences of the thermal expansion between the layer and the substrate. Despite of the presence of cracks, the wear resistance of annealed layers is still higher than the wear resistance of uncoated substrate. The analysis of the structure and properties of tungsten boride layers lead to the discussion about the application area of this material.

Keywords: hard coatings, hard materials, magnetron sputtering, mechanical properties, tungsten boride

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Authors: M. El Hajji, A. Hallaoui, L. Bazzi, A. Benlhachemi, O. Jbara, A. Tara, B. Bakiz, L. Bazzi, M. Hilali

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The objective of this study was the development of zinc-copper binary oxide "Cu2O-ZnO" thin films by the electrochemical method "cathodic electrodeposition" and their uses for the degradation of a basic dye "Congo Red" by direct anodic oxidation. The anode materials synthesized were characterized by X-ray diffraction "XRD" and by scanning electron microscopy "SEM" coupled to EDS.

Keywords: Cu2O-ZnO thin films, cathodic electrodeposition, electrodegradation, Congo Red, BDD

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Authors: D. V. S. Praneeth, V. R. Sankar Cheela, Brajesh Dubey

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Coal Combustion (CC) residues are the major by-products from thermal power plants. The disposal of ash on to land creates havoc to environment and humans. The leaching of the constituent elements pollutes ground water. Beneficiary use of coal combustion residues in structural components is being investigated as a part of this study. This application reduces stress on the convention materials in the construction industry. The present study involves determination of leaching parameters of the CC residues. Batch and column studies are performed based on Leaching Environmental Assessment Framework (LEAF) protocol. The column studies are conducted to simulate the real time percolation conditions in the field. The structural and environmental studies are performed to determine the usability of CC residues as bricks. The physical, chemical, geo environmental and mechanical properties of the alternate materials are investigated. Scanning electron microscopy (SEM), X-Ray Diffraction analysis (XRD), X-ray fluorescence (XRF) and Energy Dispersive X-ray Spectroscopy tests were conducted to determine the characteristics of CC residue ash and bricks.

Keywords: coal combustion residues, LEAF, leaching, SEM

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Authors: Alaeddine Kaouka

Abstract:

The properties and characterization of Ti-6Al-4V alloys with different contents of Mo were investigated. Microstructure characterization and hardness are considered. The alloy structure was characterized by X-ray diffraction, SEM and optical microscopy. The results showed that the addition of Mo stabilized the β-phase in the treated solution condition. The Mo element added to titanium alloys changes the lattice parameters of phases. Microstructural observations indicate an obvious reduction in the prior grain size. The hardness has increased with the increase in β-phase stability, while Young’s modulus and ductility have decreased.

Keywords: characterization, mechanical properties, molybdenum, titanium alloy

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Authors: Obsi Terfasa, Bhanupriya Das, Shiao-Shing Chen

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Converting coal fly ash (CFA) waste into ceramic membranes presents a promising alternative to traditional disposal methods, offering potential economic and environmental advantages that warrant further investigation. This research focuses on the creation of ceramic membranes exclusively from CFA using a uniaxial compaction technique. The membranes' properties were examined through various analytical methods: Scanning Electron Microscopy (SEM) revealed a porous and flawless membrane surface, X-Ray Diffraction (XRD) identified mullite and quartz crystalline structures, and Fourier-Transform Infrared Spectroscopy (FTIR) characterized the membrane's functional groups. Thermogravimetric analysis (TGA) determined the ideal sintering temperature to be 800°C. To evaluate its separation capabilities, the synthesized membrane was tested on wastewater from denim jeans production at 0.2 bar pressure. The results were impressive, with 97.42% removal of Chemical Oxygen Demand (COD), 95% color elimination, and a pure water flux of 4.5 Lm⁻²h⁻¹bar⁻¹. These findings suggest that CFA, a byproduct of thermal power plants, can be effectively repurposed to produce ultrafiltration membranes suitable for various industrial purification and separations.

Keywords: wastewater treatment, separator, coal fly ash, ceramic membrane, ultrafiltration

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Authors: Seyedeh Narjes Hosseini, Mohammad Hossein Enayati, Fathallah Karimzadeh, Nigel Mark Sammes

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The synthesis of CuFe2O4 spinel powders by an optimized combustion-like process followed by calcinations is described herein. The samples were characterized by X-ray diffraction (XRD), differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), dilatometry and 4-probe DC methods. Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48 (stoichiometric) and 2 (fuel-rich) were employed. Calcining the as-prepared powders at 800 and 1000°C for 5 hours showed that the 2 ratio results in the formation of desired copper spinel single phase at both calcinations temperatures. For G/N=1, formation of CuFe2O4 takes place in three steps. First, iron and copper nitrates decomposes to iron oxide and pure copper. Then, copper transforms to copper oxide and finally, copper and iron oxides react to each other to form copper ferrite spinel phase. The electrical conductivity and the coefficient of thermal expansion of the sintered pelletized samples were obtained 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C), respectively.

Keywords: SOFC interconnect coatings, Copper ferrite, Spinels, electrical conductivity, Glycine–nitrate process

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Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov

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The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.

Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite

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Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: Saeed Khodabakhshi, Alimorad Rashidi, Ziba Tavakoli, Sajad Kiani, Sadegh Dastkhoon

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Alumina nanoparticles (γ-Al2O3 NPs) were prepared via a new and simple synthetic route and characterized by field emission scanning electron microscope, X-ray diffraction, and Fourier transform infrared spectroscopy. The catalytic activity of prepared γ-Al2O3 NPs was investigated for the one-pot, four-component synthesis of fused tri-heterocyclic compounds containing pyrazole, pyran, and pyrimidine. This procedure has some advantages such as high efficiency, simplicity, high rate and environmental safety.

Keywords: alumina nanoparticles, one-pot, fused tri-heterocyclic compounds, pyran

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Authors: M. Veeresham

Abstract:

The microstructure, texture, phase stability, and tensile properties of annealed Ta_0.5Nb_0.5Hf_0.5ZrTi_1.5 alloy have been investigated in the present research. The alloy was severely hybrid-rolled up to 93.5% thickness reduction, subsequently rolled samples subjected to an annealing treatment at 800 °C and 1000 °C temperatures for 1 h. Consequently, the rolled condition and both annealed temperatures have a body-centered cubic (BCC) structure. Furthermore, quantitative texture measurements (orientation distribution function (ODF) analysis) and microstructural examinations (analytical electron backscatter diffraction (EBSD) maps) permitted to establish a good relationship between annealing texture and microstructure and universal testing machine (UTM) utilized for obtaining the mechanical properties. Impressive room temperature tensile properties combination with the tensile strength (1380 MPa) and (24.7%) elongation is achieved for the 800 °C heat-treated condition. The evolution of the coarse microstructure featured in the case of 1000 °C annealed temperature ascribed to the influence of high thermal energy.

Keywords: refractory high entropy alloys, hybrid-rolling, recrystallization, microstructure, tensile properties

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Authors: Radia Imane Fertout

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In recent years, the reaction of dry reforming of methane (DRM) has attracted much attention due to its environmental and industrial importance. Various catalysts, including Ni-based catalysts, have been investigated for the DRM. Doping Ni/Al₂O₃ by lanthanum and alkaline earth element may strongly influence solid-state reaction and increases the stability of catalysts due to the lower density and high basicity of these oxides. The effect of SrO on the activity and stability of Ni/Al₂O₃-La₂O₃ in dry reforming of methane was investigated. These catalysts have been prepared with the impregnation method, calcined in air at 450 and 650°C, then characterized by BET surface area, X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques and tested in DRM. The results showed that the addition of strontium to Ni/Al2O₃-La₂O₃ decreased the specific surface area. XRD results revealed the presence of different phases of Al₂O₃, La(OH)₃, La₂O₂CO₃, and SrCO₃. The catalytic evaluation results showed that adding SrO increased the catalytic activity and stability, that explained by the strong basicity of strontium. SEM analysis after the reaction indicates the formation of carbon over the spent catalyst and that the addition of strontium stabilized the surface of the catalyst.

Keywords: dry reforming of methane, Ni/Al₂O₃-La₂O₃ catalyst, strontium, nickel

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Authors: Ehsan Alishahi, Chuang Deng

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Materials with microstructural heterogeneity have recently attracted dramatic attention in the materials science community. Although most of the metals are identified as crystalline, the new class of amorphous alloys, sometimes are known as metallic glasses (MGs), exhibited remarkable properties, particularly high mechanical strength and elastic limit. The unique properties of MGs led to the wide range of studies in developing and characterizing of new alloys or composites which met the commercial desires. In spite of applicable properties of MGs, commercializing of metallic glasses was limited due to a major drawback, the lack of ductility and sudden brittle failure mode. Hence, crystalline-amorphous (C-A) composites were introduced almost in 2000s as a toughening strategy to improve the ductility of MGs. Despite the considerable progress reported in previous studies, there are still challenges in both synthesis and characterization of metallic C-A composites. In this study, accumulative roll bonding (ARB) was used to synthesize bulk crystalline-amorphous composites starting from crystalline Cu-Zr multilayers. Due to the severe plastic deformation state, new CuZr phases were formed during the rolling process which was reflected in SEM-EDS analysis. EDS elemental analysis showed the variation in the composition of CuZr phases such as 38-62, 50-50 to 68-32 at Cu-Zr % respectively. Moreover, TEM with electron diffraction analysis indicated the presence of both crystalline and amorphous structures for the new formed CuZr phases. In addition to the microstructural analysis, the mechanical properties of the synthesized composites were studied using the nanoindentation technique. Hysitron Nanoindentation instrument was used to conduct nanoindentation tests with cube corner tip. The maximum load of 5000 µN was applied in load control mode to measure the elastic modulus and hardness of different phases. The trend of results indicated three distinct regimes of hardness and elastic modulus including pure Cu, pure Zr, and new formed CuZr phases. More specifically, pure Cu regions showed the lowest values for both nanoindentation hardness and elastic modulus while the CuZr phases take the highest values. Consequently, pure Zr was placed in the intermediate range which is harder than pure Cu but softer than CuZr phases. In overall, it was found that CuZr phases with higher hardness were nucleated during ARB process as a result of mechanical alloying phenomenon.

Keywords: ARB, crystalline-amorphous composites, mechanical alloying, nanoindentation hardness

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Authors: Ahmed Farghali, Heba Amar, Mohamed Khedr

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NiAl-Layered Double Hydroxide (NiAl-LDH), one of anionic functional layered materials, has been prepared by a simple co-precipitation process. X-ray diffraction patterns confirm the formation of the desired compounds of NiAl hydroxide single phase and the crystallite size was found to be about 4.6 nm. The morphology of the prepared samples was investigated using scanning electron microscopy and the layered structure was appeared under the transmission electron microscope. The thermal stability and the function groups of NiAl-LDH were investigated using thermal gravimetric analysis (TGA) and Fourier transform infrared (FTIR) respectively. NiAl-LDH was investigated as a photo-catalyst for the degradation of some toxic dyes such as toluidine blue and bromopyrogallol red. It shows good catalytic efficiency in visible light and even in dark. For the first time NiAl-LDH was used for hydrogen storage application. NiAl-LDH samples were exposed to 20 bar applied hydrogen pressure at room temperature, 100 and -193 oC. NiAl-LDH samples appear to have feasible hydrogen storage capacity. It was capable to adsorb 0.1wt% at room temperature, 0.15 wt% at 100oC and storage capacity reached 0.3 wt% at -193 oC.

Keywords: NiAl-LDH, preparation, characterization, photo-catalysis, hydrogen storage

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Authors: K. Raza, S. Gul, M. Ali

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Concrete is a fundamental building material, extensively utilized by the construction industry. Problems related to the strength of concrete is an immense issue for the sustainability of concrete structures. Concrete mostly loses its strength due to the cracks produced in it by shrinkage or hydration process. This study aims to enhance the strength and service life of the concrete structures by incorporating bio-based admixture in the concrete. By the injection of bio-based admixture (BBA) in concrete, it will self-heal the cracks by producing calcium carbonate. Minimization of cracks will compact the microstructure of the concrete, due to which strength will increase. For this study, Bacillus subtilis will be used as a bio-based admixture (BBA) in concrete. Calcium lactate up to 1.5% will be used as the food source for the Bacillus subtilis in concrete. Two formulations containing 0 and 5% of Bacillus subtilis by weight of cement, will be used for the casting of concrete specimens. Direct mixing method will be adopted for the usage of bio-based admixture in concrete. Compressive strength test will be carried out after 28 days of curing. Scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD) will be performed for the examination of micro-structure of concrete. Results will be drawn by comparing the test results of 0 and 5% the formulations. It will be recommended to use to bio-based admixture (BBA) in concrete for columns because of the satisfactory increase in the compressive strength of concrete.

Keywords: bio-based admixture, Bacillus subtilis, calcium lactate, compressive strength

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Authors: Sh. Sohrabnezhad, A. Jafarzadeh

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In this paper, MCM-41 mesoporous material nanofibers were synthesized by an electrospinning technique. The nanofibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethyl orthosilicate (TEOS) and polyvinyl alcohol (PVA) were used as a silica source and fiber forming source, respectively. TEM and SEM images showed synthesis of MCM-41 nanofibers with a diameter of 200 nm. The pore diameter and surface area of calcined MCM-41 nanofibers was 2.2 nm and 970 m²/g, respectively. The morphology of the MCM-41 nanofibers depended on spinning voltages.

Keywords: electrospinning, electron microscopy, fiber technology, porous materials, X-ray techniques

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Authors: Dhivya Arumugam, Kaliyappan Thananjeyan

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The monomer of (3-((4-(methacryloyloxy)phenylimino)methyl)-2-hydroxybenzoic acid) schiff base polymer was prepared by reacting methacryloyl chloride with imine compound derived from 3-formylsalisylic acid and 4- aminophenol. The monomer was polymerized in DMF at 70oC using benzoyl peroxide as free radical initiator. Polymer metal complex was obtained in DMF solution of polymer with aqueous solution of metal ions. The polymer and the polymer metal complex were characterized by elemental analysis and spectral studies. The elemental analysis data suggest that the metal to ligand ratio is 1:1 and hence, it acts as a binucleating compartmental ligand. The IR spectral data of these complexes suggest that the metals are coordinated through nitrogen of the imine group, the oxygen of carboxylate ion and the oxygen of the phenolic –OH group which also acts as the bridging ligand. The electronic spectra and magnetic moments of the polychelates shows that octahedral and square planar structure for Ni(II) and Cu(II) complexes respectively. X-ray diffraction studies revealed that polychelates are highly crystalline. The thermal and electrical properties, catalytic activity, structure property relationships are discussed. Further the synthesized polymer was used for metal uptake studies from waste water, which is one of the effective waste water treatment strategies. And also, the polymers and polychelates were investigated for antimicrobial activity with various microorganisms by using agar well diffusion method and the results have been discussed.

Keywords: acyclic compartmental ligands, binucleating ligand, 3-formylsalicylic acid, free radical polymerization, polluting ions, polychelate

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Authors: M. Jalali Azizpour, H.Mohammadi Majd

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In this paper, the effect of WC-12Co particle Temperature in HVOF thermal spraying process on the coating thickness has been studied. The statistical results show that the spray distance and oxygen-to-fuel ratio are more effective factors on particle characterization and thickness of HVOF thermal spraying coatings. Spray Watch diagnostic system, scanning electron microscopy (SEM), X-ray diffraction and thickness measuring system were used for this purpose.

Keywords: HVOF, temperature, thickness, velocity, WC-12Co

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Authors: Madhan Vinu, Yue-Chun Jiang, Yi-Feng Lin, Chia-Her Lin

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An effective approach to enhance the ethanol/water pervaporation of mixed matrix membranes prepared from three microporous aluminium based metal-organic frameworks (MOFs), [Al(OH)(BPDC)] (DUT-5), [Al(OH)(NDC)] (DUT-4) and [Al(OH)(BzPDC)] (CAU-8) have been synthesized by employing solvothermal reactions. Interestingly, all Al-MOFs showed attractive surface area with microporous 12.3, 10.2 and 8.0 Å for DUT-5, DUT-4 and CAU-8 MOFs which are confirmed through N₂ gas sorption measurements. All the microporous compounds are highly stable as confirmed by thermogravimetric analysis and temperature-dependent powder X-ray diffraction measurements. Furthermore, the synthesized microporous MOF particles of DUT-5, DUT-4, and CAU-8 were successfully incorporated into biological chitosan (CS) membranes to form DUT-5@CS, DUT-4@CS, and CAU-8@CS membranes. The different MOF loadings such as 0.1, 0.15, and 0.2 wt% in CS networks have been prepared, and the same were used to separate mixtures of water and ethanol at 25ºC in the pervaporation process. In particular, when 0.15 wt% of DUT-5 was loaded, MOF@CS membrane displayed excellent permeability and selectivity in ethanol/water separation than that of the previous literature. These CS based membranes separation through functionalized microporous MOFs reveals the key governing factors that are essential for designing novel MOF membranes for bioethanol purification.

Keywords: metal-organic framework, microporous materials, separation, chitosan membranes

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Authors: Khabat M. Ahmad

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This experiment focuses on the reduction of permeability (formation damage) as a result of fines migration by changing pH and flow rate on core plugs selected from sandstone reservoir of Pannonian basin (Upper Miocene, East Hungary). The main objective of coreflooding experiments was to investigate the influence of both high and low pH fluids and the flow rate on stability of clay minerals. The selected core samples were examined by X-ray powder diffraction (XRD) for bulk mineralogical and clay mineral composition. The shape, position, distribution and type of clay minerals within the core samples were diagnosed by scanning electron microscopy and energy dispersive spectroscopy (SEM- EDS). The basic petrophysical properties such as porosity and initial permeability were determined prior to experiments. The special core analysis (influence of pH and flow rate) on permeability reduction was examined through a series of laboratory coreflooding experiments, testing for acidic (3) and alkaline (11) solutions at different flow rates (50, 100 and 200 ml/h). Permeability in continuously reduced for pH 11 to more than 50 % of initial permeability. However, at pH 3 after a slow decrease, a significant increase is observed, to more than 40 % of initial permeability. The variation is also influenced by flow rate.

Keywords: flow rate, pH, permeability, fine migration, formation damage, XRD, SEM- EDS

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Authors: Cise Unluer

Abstract:

Reactive MgO hydrates to form brucite (Mg(OH)2, magnesium hydroxide), which can then react with CO2 and additional water to form a range of strength providing hydrated magnesium carbonates (HMCs) within cement-based formulations. The presented work focuses on the use of reactive MgO in a range of concrete mixes, where it carbonates by absorbing CO2 and gains strength accordingly. The main goal involves maximizing the amount of CO2 absorbed within construction products, thereby reducing the overall environmental impact of the designed formulations. Microstructural analyses including scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetry/differential thermal analysis (TG/DTA) are used in addition to porosity, permeability and unconfined compressive strength (UCS) testing to understand the performance mechanisms. XRD Reference Intensity Ratio (RIR), acid digestion and TG/DTA are utilized to quantify the amount of CO2 sequestered, with the goal of achieving 100% carbonation through careful mix design, leading to a range of carbon neutral products with high strengths. As a result, samples stronger than those containing Portland cement (PC) were produced, revealing the link between the mechanical performance and microstructural development of the developed formulations with the amount of CO2 sequestered.

Keywords: carbonation, compressive strength, reactive MgO cement, sustainability

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Authors: Nadjet Taoualit, Zoubida Chemat, Djamel-Eddine Hadj-Boussaad

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This study aims the removal of copper Cu (II) contained in wastewater by adsorption on a perfect synthesized mud. It is the materials Hydroxides Double Lamellar, HDL, prepared and synthesized by co-precipitation method at constant pH, which requires a simple titration assembly, with an inexpensive and available material in the laboratory, and also allows us better control of the composition of the reaction medium, and gives well crystallized products. A characterization of the adsorbent proved essential. Thus a range of physic-chemical analysis was performed including: FTIR spectroscopy, X-ray diffraction… The adsorption of copper ions was investigated in dispersed medium (batch). A systematic study of various parameters (amount of support, contact time, initial copper concentration, temperature, pH…) was performed. Adsorption kinetic data were tested using pseudo-first order, pseudo-second order, Bangham's equation and intra-particle diffusion models. The equilibrium data were analyzed using Langmuir, Freundlich, Tempkin and other isotherm models at different doses of HDL. The thermodynamics parameters were evaluated at different temperatures. The results have established good potentiality for the HDL to be used as a sorbent for the removal of Copper from wastewater.

Keywords: adsoption, copper, HDL, isotherm

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Authors: Mehran Bakhshi, Mohammad Raouf Hosseini, Mohammadhosein Rahimi

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The cadmium sulfide nanoparticles were synthesized from the nickel-cadmium cake of a hydrometallurgical zinc producing plant and sodium sulfide as Cd²⁺ and S^-2 sources, respectively. Also, the synthesis process was performed by using the secretions of Bacillus licheniformis as bio-surfactant. Initially, in order to obtain a cadmium rich solution, two following steps were carried out: 1) Alkaline leaching for the removal of zinc oxide from the cake, and 2) acidic leaching to dissolve cadmium from the remained solid residue. Afterward, the obtained CdSO₄ solution was used for the nanoparticle biosynthesis. Nanoparticles were characterized by the energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) to confirm the formation of CdS crystals with cubic structure. Also, transmission electron microscopy (TEM) was applied to determine the particle sizes which were in 2-10 nm range. Moreover, the presence of the protein containing bio-surfactants was approved by using infrared analysis (FTIR). In addition, the absorbance below 400 nm confirms quantum particles’ size. Finally, it was shown that valuable CdS quantum dots could be obtained from the industrial waste products via environment-friendly biological approaches.

Keywords: biosynthesis, cadmium cake, cadmium sulfide, nanoparticle, zinc smelter

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Authors: Laila Mahtout, Kerami Ahmed, Rabhi Souhila

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The objective of this work is to reduce the impact on the environment of an acid dye (Black Eriochrome T) using catalytic photo-degradation in the presence of the semiconductor powder (TiO₂) previously characterized. A series of tests have been carried out in order to demonstrate the influence of certain parameters on the degree of dye degradation by titanium dioxide in the presence of UV rays, such as contact time, the powder mass and the pH of the solution. X-ray diffraction analysis of the powder showed that the anatase structure is predominant and the rutile phase is presented by peaks of low intensity. The various chemical groups which characterize the presence of the bands corresponding to the anatase and rutile form and other chemical functions have been detected by the Fourier Transform Infrared spectroscopy. The photo degradation of the NET by TiO₂ is very interesting because it gives encouraging results. The study of photo-degradation at different concentrations of the dye showed that the lower concentrations give better removal rates. The degree of degradation of the dye increases with increasing pH; it reaches the maximum value at pH = 9. The ideal mass of TiO₂ which gives the high removal rate is 1.2 g/l. Thermal treatment of TiO₂ with the addition of CuO with contents of 5%, 10%, and 15% respectively gives better results of degradation of the NET dye. The high percentage of elimination is observed at a CuO content of 15%.

Keywords: acid dye, ultraviolet rays, degradation, photocatalyse

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Authors: Pimchanok Puksisuwan, Pitak Laorattanakul, Benya Cherdhirunkorn

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The use of aluminium dross as a raw material for geopolymer synthesis via mechanochemistry method was studied. The geopolymers were prepared using aluminium dross from secondary aluminium industry, fly ash from a biomass power plant and liquid alkaline activators, which is a mixture of sodium silicate solution (Na2SiO3) and sodium hydroxide solution (NaOH) (Na2SiO3/NaOH ratio 4:1, 3:1 and 2:1). Aluminium dross consists mostly of alumina (Al2O3), silicon oxide (SiO2) and aluminium nitride (AlN). The raw materials were mixed and milled using the high energy ball milling method for 5, 10 and 15 minutes in order to reduce the particle size. The milled powders were uniaxially pressed into a cylinder die with the pressure of 2200 psi. The cylinder samples were cured in the sealed plastic bags for 3, 7 and 14 days at the room temperature and 60°C for 24 hour. The mechanical property of geopolymers was investigated. In addition, scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis were carried out in order to study the microstructure and phase structures of the geopolymers, respectively. The results showed that aluminium dross could enhance the mechanical property of geopolymers product by mechanochemistry method and meet the TISI requirements.

Keywords: aluminium dross, fly ash, geopolymer, mechanochemistry

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Authors: Princess Stephanie P. Llanos, Rinlee Butch M. Cervera

Abstract:

Lithium iron phosphate (LiFePO4) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, carbon-coated nanograined LiFePO4 is synthesized via wet chemistry method at a low temperature of 400 °C and investigated its performance as a cathode in Lithium battery. The X-ray diffraction pattern of the synthesized samples can be indexed to an orthorhombic LiFePO4 structure. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LiFePO4 and coating of amorphous carbon layer. Elemental mapping using Energy dispersive spectroscopy analysis revealed the homogeneous dispersion of Fe, P, O, and C elements. On the other hand, the electrochemical performances of the synthesized cathodes were investigated using cyclic voltammetry, galvanostatic charge/discharge tests with different C-rates, and cycling performances. Galvanostatic charge and discharge measurements revealed that the sample sintered at 400 °C for 3 hours with carbon coating demonstrated the highest capacity among the samples which reaches up to 160 mAhg⁻¹ at 0.1C rate.

Keywords: cathode, charge-discharge, electrochemical, lithium batteries

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Authors: Amina Adala, Nadra Debbache, Tahar Sehili

Abstract:

Coordination polymers and uniformly {[Zn(II)(BIPY)(Pht)]n} (1), {[Zn (HYD)(Pht)]n} (2) (BIPY = 4,4’ bipyridine, Pht = terephtalic acid, HYD = 8-hydroxyquinoline) have been successfully synthesized by a hydrothermal process using aqueous zinc solution. The as-prepared compounds phases were characterized by X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy, UV-visible spectroscopy, thermogravimetric analysis (TGA), and the electrochemistry study by the voltammetry cyclic. The results showed a crystalline phase for CP1 however, CP2 requires recrystallization; the FTIR showed the presence of characteristic bands of all ligands; besides that, TGA shows thermal stability up to 300°C. The electrochemistry study showed a good charge transfer between the ligands and Zn metal for the two components. UV-Vis measurement showed strong absorption in a wide range from UV to visible light with a band gap of 2.69 eV for CP1 and 2.56 eV for CP2, smaller than that of ZnO. This represents an alternative to using ZnO. The Ibuprofen IBP decomposition kinetics of 5.10⁻⁵ mol.L⁻¹ under solar and artificial light were studied for different irradiation conditions. Good photocatalytic properties were observed due to their high surface area.

Keywords: metal-organic frameworks, photocatalysis, photodegradation, organic pollutant, ibuprofen

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Authors: Mohamed dammak

Abstract:

Great attention has been paid to the design and synthesis of novel organic-inorganic compounds in recent decades because of their structural variety and the large diversity of atomic arrangements. In this work, the structure for the novel dimethyl aminopyridine tetrachlorocobaltate (C₇H₁₁N₂)₂CoCl₄ prepared by the slow evaporation method at room temperature has been successfully discussed. The X-ray diffraction results indicate that the hybrid material has a triclinic structure with a P space group and features a 0D structure containing isolated distorted [CoCl₄]2- tetrahedra interposed between [C7H11N²⁻]+ cations forming planes perpendicular to the c axis at z = 0 and z = ½. The effect of the synthesis conditions and the reactants used, the interactions between the cationic planes, and the isolated [CoCl4]2- tetrahedra are employing N-H...Cl and C-H…Cl hydrogen bonding contacts. The inspection of the Hirshfeld surface analysis helps to discuss the strength of hydrogen bonds and to quantify the inter-contacts. A phase transition was discovered by thermal analysis at 390 K, and comprehensive dielectric research was reported, showing a good agreement with thermal data. Impedance spectroscopy measurements were used to study the electrical and dielectric characteristics over a wide range of frequencies and temperatures, 40 Hz–10 MHz and 313–483 K, respectively. The Nyquist plot (Z" versus Z') from the complex impedance spectrum revealed semicircular arcs described by a Cole-Cole model. An electrical circuit consisting of a link of grain and grain boundary elements is employed. The real and imaginary parts of dielectric permittivity, as well as tg(δ) of (C₇H₁₁N₂)₂CoCl₄ at different frequencies, reveal a distribution of relaxation times. The presence of grain and grain boundaries is confirmed by the modulus investigations. Electric and dielectric analyses highlight the good protonic conduction of this material.

Keywords: organic-inorganic, phase transitions, complex impedance, protonic conduction, dielectric analysis

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Authors: Ramovatar, Neeraj Panwar

Abstract:

Lead free Ba₀.₉₈Ca₀.₀₂SnxTi₁₋ₓO₃ (x = 0.01 and 0.05 mole %) ferroelectric ceramics have been synthesized by the solid-state reaction method with sintering at 1400 °C for 2 h. The room temperature x-ray diffraction (XRD) patterns identified the tetragonal phase for x = 0.01 composition whereas co-existence of tetragonal and orthorhombic phases for x =0.05 composition. Raman spectroscopy results corroborated with the XRD results at room temperature. The maximum dielectric properties (ɛm ~ 8591, tanδ ~ 0.018) were obtained for the compound with x = 0.01 at 5 kHz. Further, the tetragonal to cubic (TC) transition temperature was observed at 122 °C and 102 °C for the ceramics with x =0.01 and x = 0.05, respectively. The temperature dependent P-E loops also revealed the existence of TC at these particular temperature values. The energy storage density (Ed) of both compounds was calculated from room temperature P – E loops at an applied electric field of 20 kV/cm. The maximum Ed ~ 224 kJ/m³ was achieved for the sample with x = 0.01 as compared to 164 kJ/m³ for the x =0.05 composition. The value of Ed is comparable to other BaTiO₃ based lead free ferroelectric systems. Impedance spectroscopy analysis exhibited the bulk and grain boundary contributions above 300 °C under the frequency range 100 Hz to 1 MHz. The above properties make these ceramics suitable for energy storage devices.

Keywords: dielectric properties, energy storage properties, impedance spectroscopy, lead free ceramics

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