Search results for: nickel oxides

Authors: B. Pavan Kumar Reddy, P. Michael Preetam Raj, Souri Banerjee, Souvik Kundu

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In this work, the fabrication and characterization of copper-doped zinc oxide (Cu:ZnO) based memristor devices with aluminum (Al) and indium tin oxide (ITO) metal electrodes are reported. The thin films of Cu:ZnO was synthesized using low-cost and low-temperature chemical process. The Cu:ZnO was then deposited onto ITO bottom electrodes using spin-coater technique, whereas the top electrode Al was deposited utilizing physical vapor evaporation technique. Ellipsometer was employed in order to measure the Cu:ZnO thickness and it was found to be 50 nm. Several surface and materials characterization techniques were used to study the thin-film properties of Cu:ZnO. To ascertain the efficacy of Cu:ZnO for memristor applications, electrical characterizations such as current-voltage (I-V), data retention and endurance were obtained, all being the critical parameters for next-generation memory. The I-V characteristic exhibits switching behavior with asymmetrical hysteresis loops. This work imputes the resistance switching to the positional drift of oxygen vacancies associated with respect to the Al/Cu:ZnO junction. Further, a non-linear curve fitting regression techniques were utilized to determine the equivalent circuit for the fabricated Cu:ZnO memristors. Efforts were also devoted in order to establish its potentiality for different electronic applications.

Keywords: copper doped, metal-oxides, oxygen vacancies, resistive switching

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Authors: I. Sinnarasa, Y. Thimont, L. Presmanes, A. Barnabé

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The thermoelectricity is a promising technique to overcome the issues in recovering waste heat to electricity without using moving parts. In fact, the thermoelectric (TE) effect defines as the conversion of a temperature gradient directly into electricity and vice versa. To optimize TE materials, the power factor (PF = σS² where σ is electrical conductivity and S is Seebeck coefficient) must be increased by adjusting the carrier concentration, and/or the lattice thermal conductivity Kₜₕ must be reduced by introducing scattering centers with point defects, interfaces, and nanostructuration. The PF does not show the advantages of the thin film because it does not take into account the thermal conductivity. In general, the thermal conductivity of the thin film is lower than the bulk material due to their microstructure and increasing scattering effects with decreasing thickness. Delafossite type oxides CuᴵMᴵᴵᴵO₂ received main attention for their optoelectronic properties as a p-type semiconductor they exhibit also interesting thermoelectric (TE) properties due to their high electrical conductivity and their stability in room atmosphere. As there are few proper studies on the TE properties of Mg-doped CuCrO₂ thin films, we have investigated, the influence of the annealing temperature on the electrical conductivity and the Seebeck coefficient of Mg-doped CuCrO₂ thin films and calculated the PF in the temperature range from 40 °C to 220 °C. For it, we have deposited Mg-doped CuCrO₂ thin films on fused silica substrates by RF magnetron sputtering. This study was carried out on 300 nm thin films. The as-deposited Mg doped CuCrO₂ thin films have been annealed at different temperatures (from 450 to 650 °C) under primary vacuum. Electrical conductivity and Seebeck coefficient of the thin films have been measured from 40 to 220 °C. The highest electrical conductivity of 0.60 S.cm⁻¹ with a Seebeck coefficient of +329 µV.K⁻¹ at 40 °C have been obtained for the sample annealed at 550 °C. The calculated power factor of optimized CuCrO₂:Mg thin film was 6 µW.m⁻¹K⁻² at 40 °C. Due to the constant Seebeck coefficient and the increasing electrical conductivity with temperature it reached 38 µW.m⁻¹K⁻² at 220 °C that was a quite good result for an oxide thin film. Moreover, the degenerate behavior and the hopping mechanism of CuCrO₂:Mg thin film were elucidated. Their high and constant Seebeck coefficient in temperature and their stability in room atmosphere could be a great advantage for an application of this material in a high accuracy temperature measurement devices.

Keywords: thermoelectric, oxides, delafossite, thin film, power factor, degenerated semiconductor, hopping mode

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Authors: G. Nyongombe, Guy L. Kabongo, B. M. Mothudi, M. S. Dhlamini

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A series of Transition Metals Oxides (TMOs) doped graphene were synthesized and successfully used as supercapacitor electrode materials. The as-synthesized materials exhibited exceptional electrochemical properties owing to the combined properties of its constituents; high surface area and good conductivity were achieved. Several analytical characterization techniques were employed to investigate the morphology, crystal structure atomic arrangement and elemental chemical state in the materials for which scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were conducted, respectively. Moreover, the electrochemical properties of the as-synthesized materials were examined by performing cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) measurements. Furthermore, the effect of doping concentration on the interlayer distance of the graphene materials and the charge transfer resistance are investigated and correlated to the exceptional current density which was multiplied by a factor of ~80 after TMOs doping in graphene. Finally, the resulting high capacitance obtained confirms the contribution of grapheme exceptional electronic conductivity and large surface area on the electrode materials. Such good-performing electrode materials are highly promising for supercapacitors and other energy storage devices.

Keywords: energy density, graphene, supercapacitors, TMOs

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Authors: H. Boucheloukh, S. Rouissa, N. Aoun, M. Beloucifa, T. Sehili, F. Parrino, V. Loddo

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To optimize water purification and wastewater treatment by heterogeneous photocatalysis, we used NiFe₂O₄ as a catalyst and solar irradiation as a source of energy. In this concept, an organic substance present in many industrial effluents was chosen: naproxen ((S)-6-methoxy-α-methyl-2-naphthaleneacetic acid or 2-(6-methoxynaphthalenyl) propanoic), a non-steroidal anti-inflammatory drug. The main objective of this study is to degrade naproxen by an iron and nickel catalyst, the degradation of this organic pollutant by nickel ferrite has been studied in a heterogeneous aqueous medium, with the study of the various factors influencing photocatalysis such as the concentration of matter and the acidity of the medium. The photocatalytic activity was followed by HPLC-UV andUV-Vis spectroscopy. A first-order kinetic model appropriately fitted the experimental data. The degradation of naproxen was also studied in the presence of H₂O₂ as well as in an aqueous solution. The new hetero-system NiFe₂O₄/oxalic acid is also discussed. The fastest naproxen degradation was obtained with NiFe₂O₄/H₂O₂. In a first-place, we detailed the characteristics of the material NiFe₂O₄, which was synthesized by the sol-gel methods, using various analytical techniques: visible UV spectrophotometry, X-ray diffraction, FTIR, cyclic voltammetry, luminescent discharge optical emission spectroscopy.

Keywords: naproxen, nickelate, photocatalysis, oxalic acid

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Authors: Mulatu Kassie Birhanu

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Electro-oxidation of glycerol is an important process to convert the less price glycerol into other expensive (essential) and energy-rich chemicals. In this study, nickel was electro-deposited on laboratory-made carbon ceramic electrode (CCE) substrate using electrochemical techniques that is cyclic voltammetry (CV) to prepare an electro-catalyst (Ni/CCE) for electro-oxidation of glycerol. Carbon ceramic electrode was prepared from graphite and methyl tri-methoxy silane (MTMOS) through the processes called hydrolysis and condensation with methanol in acidic media (HCl) by a sol-gel technique. Physico-chemical characterization of bare CCE and modified (deposited) CCE (Ni/CCE) was measured and evaluated by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). Electro-oxidation of glycerol was performed in 0.1 M glycerol in alkaline media (0.5 M NaOH). High-Performance Liquid Chromatography (HPLC) technique was used to identify and determine the concentration of glycerol, reaction intermediates and oxidized products of glycerol after its electro-oxidation is performed. The conversion (%) of electro-oxidation of glycerol during 9-hour oxidation was 73% and 36% at 1.8V and 1.6V vs. RHE, respectively. Formate, oxalate, glycolate and glycerate are the main oxidation products of glycerol with selectivity (%) of 75%, 8.6%, 1.1% and 0.95 % at 1.8 V vs. RHE and 55.4%, 2.2%, 1.0% and 0.6% at 1.6 V vs. RHE respectively. The result indicates that formate is the main product in the electro-oxidation of glycerol on Ni/CCE using the indicated applied potentials.

Keywords: carbon-ceramic electrode, electrodeposition, electro-oxidation, Methyltrimethoxysilane

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Authors: Haifa El-Sadi, Maria Elektorowicz, Reed Rushing, Ammar Badawieh, Asif Chaudry

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Clay soils have particular properties that affect the assessment and remediation of contaminated sites. In clay soils, electro-kinetic transport of heavy metals has been carried out. The transport of these metals is predicated on maintaining a low pH throughout the cell, which, in turn, keeps the metals in the pore water phase where they are accessible to electro-kinetic transport. Supercritical fluid extraction and acid digestion were used for the analysis of heavy metals concentrations after the completion of electro-kinetic experimentation. Supercritical fluid (carbon dioxide) extraction is a new technique used to extract the heavy metal (lead, nickel, calcium and potassium) from clayey soil. The comparison between supercritical extraction and acid digestion of different metals was carried out. Supercritical fluid extraction, using ethylenediaminetetraacetic acid (EDTA) as a modifier, proved to be efficient and a safer technique than acid digestion technique in extracting metals from clayey soil. Mixing time of soil with EDTA before extracting heavy metals from clayey soil was investigated. The optimum and most practical shaking time for the extraction of lead, nickel, calcium and potassium was two hours.

Keywords: clay soil, heavy metals, supercritical fluid extraction, acid digestion

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Authors: Abdel Ghany F. Shoair, Mai M. A. H. Shanab

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The basic aqueous systems NiSO4.6H₂O / K₂S₂O₈ (PH= 14) or NiSO₄.6H₂O / KBrO₃ (PH = 11.5) were ‎investigated ‎for the ‎catalytic conversion benzyl alcohol and ‎some para-substituted benzyl ‎alcohols to their ‎corresponding ‎acids in 75-97 % yield at room ‎temperature. The active species ‎was isolated and characterized by scanning ‎electron ‎microscopy (SEM), ‎‎transmission electron microscopy (TEM), X-ray ‎powder diffraction, EDX and ‎‎FT-IR ‎techniques and identified as NiO₂ nanoparticles (NPNPs). The SEM and ‎TEM images of nickel peroxide samples show a fine spherical-like ‎aggregation of ‎NiO₂ molecules with a nearly homogeneous partial size and confirm the ‎aggregation's size ‎to ‎be in the range of 2-3 nm. The yields, turnover (TO) and turn ‎over frequencies (TOF) were calculated. ‎It was noticed ‎that the aromatic alcohols ‎containing para-substituted electron donation groups gave better ‎‎yields than ‎those having electron-withdrawing groups. The optimum conditions for this ‎‎catalytic reaction ‎were studied using benzyl alcohol as a model. The mechanism ‎of the ‎catalytic conversion reaction was ‎suggested, in which the produced ‎(NPNPs) convert alcohols ‎to acids in two steps through the formation of the ‎‎corresponding aldehyde. The produced ‎NiO, because of this conversion, is ‎converted again to (NPNPs) by ‎an excess of K₂S₂O₈ or KBrO₃. This ‎catalytic cycle continues ‎until all the substrate is oxidized.

Keywords: Nickel, oxidation, catalysts, benzyl alcohol

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Authors: Gökhan Polat, Dicle Kocaoğlu Yılmazer, Muhlis Nezihi Sarıdede

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Iron oxides are the main input to produce iron in integrated iron and steel plants. During production of iron from iron oxides, some wastes with high iron content occur. These main wastes can be classified as basic oxygen furnace (BOF) sludge, flue dust and rolling scale. Recycling of these wastes has a great importance for both environmental effects and reduction of production costs. In this study, recycling experiments were performed on basic oxygen furnace sludge, flue dust and rolling scale which contain 53.8%, 54.3% and 70.2% iron respectively. These wastes were mixed together with coke as reducer and these mixtures are pressed to obtain cylindrical briquettes. These briquettes were pressed under various compacting forces from 1 ton to 6 tons. Also, both stoichiometric and twice the stoichiometric cokes were added to investigate effect of coke amount on reduction properties of the waste mixtures. Then, these briquettes were reduced at 1000°C and 1100°C during 30, 60, 90, 120 and 150 min in a muffle furnace. According to the results of reduction experiments, the effect of compacting force, temperature and time on reduction ratio of the wastes were determined. It is found that 1 ton compacting force, 150 min reduction time and 1100°C are the optimum conditions to obtain reduction ratio higher than 75%.

Keywords: Coke, iron oxide wastes, recycling, reduction

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Authors: Mohd Kamil Vakil

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Air Pollution is caused by the introduction of chemicals in the biosphere. Primary pollutants on reaction with the components of the earth produce Secondary Pollutants like Smog. Ozone is the main ingredient of Smog. The ground level ozone is created by the chemical reactions between Nitrogen Oxides (NOx) and Volatile Organic Compounds (VOCs) in the presence of Sunlight. This ozone can enter inside and call as indoor ozone. The automobile emissions in both moving and idling conditions contribute to the indoor ozone formation. During engine ignition and shutdown, motor vehicles emit the ozone forming pollutants like NOx and VOCs, and the phenomena are called Cold Start and Hot-Soak respectively. Subjects like Chronic Obstructive Pulmonary Disease (COPD) and asthma associated with chronic respiratory diseases are susceptible to the harmful effects of Indoor Ozone. The most common cause of COPD other than smoking is the long-term contract with harmful pollutants like ground-level ozone. It is estimated by WHO that COPD will become the third leading cause of all deaths worldwide by 2030. In this paper, the cold-start and hot-soak vehicle emissions are studied in the context of accumulation of oxides of nitrogen at the outer walls of the building which may cause COPD. The titanium oxide coated building material is further discussed as an absorber of NOx when applied to the walls and roof.

Keywords: indoor air quality, cold start emission, hot-soak, ozone

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Authors: Girish Sambhaji Gund

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The controlled nanostructure growth and its strong coupling with the current collector are key factors to achieve good electrochemical performance of faradaic-dominant electroactive materials. We employed binder-less and additive-free hydrothermal and physical vapor doping methods for the synthesis of nickel (Ni) and cobalt (Co) based compounds nanostructures (NiO, NiCo2O4, NiCo2S4) deposited on different conductive substrates such as carbon nanotube (CNT) on stainless steel, and reduced graphene oxide (rGO) and N-doped rGO on nickel foam (NF). The size and density of Ni- and Co-based compound nanostructures are controlled through the strong coupling with carbon allotropes on stainless steel and NF substrates. This controlled nanostructure of Ni- and Co-based compounds with carbon allotropes leads to stable faradaic electrochemical reactions at the material/current collector interface and within the electrode, which is consequence of strong coupling of nanostructure with functionalized carbon surface as a buffer layer. Thus, it is believed that the results provide the synergistic approaches to stabilize electrode materials physically and chemically, and hence overall electrochemical activity of faradaic dominating battery-type electrode materials through buffer layer engineering.

Keywords: metal compounds, carbon allotropes, doping, electrochemicstry, hybrid supercapacitor

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Authors: Ben Yahia Nouha, Harris Chris, Boussen Slim, Chaabani Fredj

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The present work has set itself the objective of studying non-detritic siliceous rocks in the extreme northwestern of Tunisia. It aims to discuss the origin and depositional environment of siliceous rocks based on petrographic, mineralogical, and geochemical results. The different sections were made in the area of Babouch and the area of Cap-Serrat. The collected samples were subjected to petrographic, mineralogical, and geochemical characterization using different analytical methods: scanning electron microscopy (SEM), X-ray diffraction (XRD), geochemical analysis (ICP- AES), isotopic geochemistry (δ¹⁸O) to assess their suitability for industrial use. These babouchite shows that the mineralogy consists of quartz as the dominant mineral with the total lack of amorphous silica, while clay represents the minor phase. The petrographic examination revealed allowed to deduce that it is a rock of chemical origin deriving from tests of siliceous organisms (the radiolarians). Chemical analyzes show that SiO₂, Al₂O₃, and Fe₂O₃ represent the most abundant oxides. The other oxides are present in negligible quantity. Geochemical data support a biogenic and non-hydrothermal origin of babouchite silica. Oxygen isotopic has shown that babouchites are formed in an environment with a high temperature, ranging from 56°C to 73°C.

Keywords: siliceous rocks, babouchite formation, XRD, chemical analysis, isotopic geochemistry, Northwestern of Tunisia

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Authors: Nour El Houda Bensiradj, Nafila Zouaghi, Taha Bensiradj

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The pollution of water resources is characterized by the presence of microorganisms, chemicals, or industrial waste. Generally, this waste generates effluents containing large quantities of heavy metals, making the water unsuitable for consumption and causing the death of aquatic life and associated biodiversity. Currently, it is very important to assess the impact of heavy metals in water pollution as well as the processes for treating and reducing them. Among the methods of water treatment and disinfection, we mention the complexation of metal ions using ligands which serve to precipitate and subsequently eliminate these ions. In this context, we are interested in the study of complexes containing heavy metals such as zinc, nickel, and cadmium, which are present in several industrial discharges and are discharged into water sources. We will use the ligands of triethanolamine (TEA) and nitrilotriacetic acid (NTA). The theoretical study is based on molecular modeling, using the density functional theory (DFT) implemented in the Gaussian 09 program. The geometric and energetic properties of the above complexes will be calculated. Spectral properties such as infrared, as well as reactivity descriptors, and thermodynamic properties such as enthalpy and free enthalpy will also be determined.

Keywords: heavy metals, NTA, TEA, DFT, IR, reactivity descriptors

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Authors: K. L. Pan, M. B. Chang

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Nitrogen oxides (NOₓ) is regarded as one of the most important air pollutants. It not only causes adverse environmental effects but also harms human lungs and respiratory system. As a post-combustion treatment, selective catalytic reduction (SCR) possess the highest NO removal efficiency ( ≥ 85%), which is considered as the most effective technique for removing NO from gas streams. However, injection of reducing agent such as NH₃ is requested, and it is costly and may cause secondary pollution. Reduction of NO with carbon monoxide (CO) as reducing agent has been previously investigated. In this process, the key step involves the NO adsorption and dissociation. Also, the high performance mainly relies on the amounts of oxygen vacancy on catalyst surface and redox ability of catalyst, because oxygen vacancy can activate the N-O bond to promote its dissociation. Additionally, perfect redox ability can promote the adsorption of NO and oxidation of CO. Typically, noble metals such as iridium (Ir), platinum (Pt), and palladium (Pd) are used as catalyst for the reduction of NO with CO; however, high cost has limited their applications. Recently, transition metal oxides have been investigated for the reduction of NO with CO, especially CuₓOy, CoₓOy, Fe₂O₃, and MnOₓ are considered as effective catalysts. However, deactivation is inevitable as oxygen (O₂) exists in the gas streams because active sites (oxygen vacancies) of catalyst are occupied by O₂. In this study, Cu-Ce-Fe-Co is prepared and supported on activated carbon by impregnation method to form 10% wt. Cu-Ce-Fe-Co/activated carbon catalyst. Generally, addition of activated carbon on catalyst can bring several advantages: (1) NO can be effectively adsorbed by interaction between catalyst and activated carbon, resulting in the improvement of NO removal, (2) direct NO decomposition may be achieved over carbon associated with catalyst, and (3) reduction of NO could be enhanced by a reducing agent over carbon-supported catalyst. Therefore, 10% wt. Cu-Ce-Fe-Co/activated carbon may have better performance for reduction of NO with CO. Experimental results indicate that NO conversion achieved with 10% wt. Cu-Ce-Fe-Co/activated carbon reaches 83% at 150°C with 300 ppm NO and 10,000 ppm CO. As temperature is further increased to 200°C, 100% NO conversion could be achieved, implying that 10% wt. Cu-Ce-Fe-Co/activated carbon prepared has good activity for the reduction of NO with CO. In order to investigate the effect of O₂ on reduction of NO with CO, 1-5% O₂ are introduced into the system. The results indicate that NO conversions still maintain at ≥ 90% with 1-5% O₂ conditions at 200°C. It is worth noting that effect of O₂ on reduction of NO with CO could be significantly improved as carbon is used as support. It is inferred that carbon support can react with O₂ to produce CO₂ as O₂ exists in the gas streams. Overall, 10% wt. Cu-Ce-Fe-Co/activated carbon is demonstrated with good potential for reduction of NO with CO, and possible mechanisms will be elucidated in this paper.

Keywords: nitrogen oxides (NOₓ), carbon monoxide (CO), reduction of NO with CO, carbon material, catalysis

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements

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Authors: Ben Yahia Nouha, Harris Chris, Sebei Abdelaziz, Boussen Slim, Chaabani Fredj

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The present work has set itself the objective of studying non-detritic siliceous rocks of the extreme northwest Tunisia. It aims to examine the origin and their sedimentary depositional environment based on mineralogical and geochemical characteristics. The different sections were located in the area of Babouch and the area of Tabarka. The collected samples were subjected to mineralogical and geochemical characterization using different analytical methods: X-ray diffraction (XRD), geochemical analysis (ICP- AES), isotopic geochemistry (δ18O), to assess their suitability for industrial use. X-ray powder diffraction of the pure siliceous rock indicates quartz as the major mineral, with the total lack of amorphous silica. Trace impurities, such as carbonate and clay minerals, are concealed in the analytical results. The petrographic examination revealed allowed us to deduce that this rock was deriving from tests of siliceous organisms (the radiolarians). The chemical composition shows that SiO2, Al2O3, and Fe2O3 represent the most abundant oxides. The other oxides are present in negligible quantities. Geochemical data support a biogenic and non-hydrothermal origin of babouchite silica. Oxygen isotopic has shown that babouchites were formed in an environment with a high temperature ranging from 56 °C to 73 °C.

Keywords: biogenic silica, babouchite formation, XRD, chemical analysis, oxygen isotopic, northwest tunisia

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Authors: Tatiana S. Ogneva

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Aluminum and nickel-based intermetallic compounds have attracted the attention of scientific community as promising materials for heat-resistant and wear-resistant coatings in such manufacturing areas as microelectronics, aircraft and rocket building and chemical industries. Magnetron sputtering makes possible to coat materials without formation of liquid phase and improves the mechanical and functional properties of nickel aluminides due to the possibility of nanoscale structure formation. The purpose of the study is the investigation of structure and properties of intermetallic coatings produced by magnetron sputtering technique. The feature of this work is the using of composite targets for sputtering, which were consisted of two semicircular sectors of cp-Ni and cp-Al. Plates of alumina, silicon, titanium and steel alloys were used as substrates. To estimate sputtering conditions on structure of intermetallic coatings, a series of samples were produced and studied in detail using scanning and transition electron microcopy and X-Ray diffraction. Besides, nanohardness and scratching tests were carried out. The varying parameters were the distance from the substrate to the target, the duration and the power of the sputtering. The thickness of the obtained intermetallic coatings varied from 0.05 to 0.5 mm depending on the sputtering conditions. The X-ray diffraction data indicated that the formation of intermetallic compounds occurred after sputtering without additional heat treatment. Sputtering at a distance not closer than 120 mm led to the formation of NiAl phase. Increase in the power of magnetron from 300 to 900 W promoted the increase of heterogeneity of the phase composition and the appearance of intermetallic phases NiAl, Ni₂Al₃, NiAl₃, and Al under the aluminum side, and NiAl, Ni₃Al, and Ni under the nickel side of the target. A similar trend is observed with increasing the distance of sputtering from 100 to 60 mm. The change in the phase composition correlates with the changing of the atomic composition of the coatings. Scanning electron microscopy revealed that the coatings have a nanoscale grain structure. In this case, the substrate material and the distance from the substrate to the magnetron have a significant effect on the structure formation process. The size of nanograins differs from 10 to 83 nm and depends not only on the sputtering modes but also on material of a substrate. Nanostructure of the material influences the level of mechanical properties. The highest level of nanohardness of the coatings deposited during 30 minutes on metallic substrates at a distance of 100 mm reached 12 GPa. It was shown that nanohardness depends on the grain size of the intermetallic compound. Scratching tests of the coatings showed a high level of adhesion of the coating to substrate without any delamination and cracking. The results of the study showed that magnetron sputtering of composite targets consisting of nickel and aluminum semicircles makes it possible to form intermetallic coatings with good mechanical properties directly in the process of sputtering without additional heat treatment.

Keywords: intermetallic coatings, magnetron sputtering, mechanical properties, structure

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Authors: Sabiha Chouchane, Azzedine Hani, Jean-Paul Chopart, Alexandra Levesque

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The electrodeposition of Zn-Ni alloy is mostly studied for its high degree of corrosion and mechanical properties. In this work, the zinc–nickel alloy coatings elaborated from sulfate bath have been carried out under low and high applied magnetic field. The effect of alloy stuctural parameters upon corrosion behavior is studied. It has been found that the magnetically induced convection changes the phase composition, promoting the zinc phase in spite of the γ-Ni₅Zn₂₁. Low magnetic field acts also on the morphology of the deposits as a levelling agent and a refiner by lowering the deposit roughness Ra and the spot size. For alloy obtained with low magnetic field (up to 1T) superimposition, surface morphology modification has no significant influence on corrosion behavior whereas for low nickel content alloy, the modification of phase composition, induced by applied magnetic field, favours higher polarization resistance. When high magnetic field amplitude is involved (up to12T), the phase composition modifications are the same that for low applied B and the morphology is not largely modified. In this case, the hydrogen reduction current dramatically decreases that leads to a large shift of the corrosion potential. It is suggested that the surface reactivity of electrodeposited alloys depends on the magnetically induced convection that is efficient during the codeposition process.

Keywords: magnetic field, Zn-Ni alloy, corrosion, corrosive medium

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Authors: Fadwa Chtioui

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The field of endodontics has witnessed constant advancements in treatment methods and instrument design, particularly for nickel-titanium (NiTi) files. Despite these developments, it remains crucial for clinicians to have a thorough understanding of their characteristics and behavior to choose the appropriate instruments for different clinical and anatomical situations. Research Aim: The aim of this work is to study and discuss the impact of heat treatment developments on the properties of endodontic NiTi files, with the ultimate goal of providing ways to adapt these files to the anatomical features of dental roots. Methodology: This study involves both clinical cases and extensive bibliographic research. Findings: The study highlights the importance of heat treatment in the design and manufacture of NiTi files, as it significantly affects their physical and mechanical properties. It also provides insights into the ways in which NiTi files can be adapted to the complex geometries of dental roots for more effective endodontic treatments. Theoretical Importance: Theoretical implications of this study include a better understanding of the relationship between heat treatment and the properties of NiTi files, leading to improvements in both their manufacturing methods and clinical applications. Data Collection and Analysis Procedures: The data for this study was collected through clinical cases and an extensive review of relevant literature. Analysis was performed through qualitative and quantitative methods, examining the impact of heat treatment on the physical and mechanical properties of NiTi files. Questions Addressed: This study aims to answer questions concerning the properties of NiTi files and the impact of heat treatment on their behavior. It also seeks to examine ways in which these files can be adapted to complex dental root geometries for more effective endodontic treatments. Conclusion: In conclusion, this study emphasizes the importance of heat treatment in the design and manufacture of NiTi files, as it significantly impacts their physical and mechanical properties. Further research is necessary to explore additional methods for adapting NiTi files to the unique anatomies of dental roots to improve endodontic treatments further. Ultimately, this study provides valuable insights into the continued evolution of endodontic treatment and instrument design.

Keywords: endodontic files, nickel-titanium, tooth anatomy, heat treatment

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Authors: D. Varadaradjou, H. Kebir, J. Mespoulet, D. Tingaud, S. Bouvier, P. Deconick, K. Ameyama, G. Dirras

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The development of new architecture metallic alloys with controlled microstructures is one of the strategic ways for designing materials with high innovation potential and, particularly, with improved mechanical properties as required for structural materials. Indeed, unlike conventional counterparts, metallic materials having so-called harmonic structure displays strength and ductility synergy. The latter occurs due to a unique microstructure design: a coarse grain structure surrounded by a 3D continuous network of ultra-fine grain known as “core” and “shell,” respectively. In the present study, pure harmonic-structured (HS) Nickel samples were processed via controlled mechanical milling and followed by spark plasma sintering (SPS). The present work aims at characterizing the mechanical properties of HS pure Nickel under room temperature dynamic loading through a Split Hopkinson Pressure Bar (SHPB) test and the underlying microstructure evolution. A stopper ring was used to maintain the strain at a fixed value of about 20%. Five samples (named B1 to B5) were impacted using different striker bar velocities from 14 m/s to 28 m/s, yielding strain rate in the range 4000-7000 s-1. Results were considered until a 10% deformation value, which is the deformation threshold for the constant strain rate assumption. The non-deformed (INIT – post-SPS process) and post-SHPB microstructure (B1 to B5) were investigated by EBSD. It was observed that while the strain rate is increased, the average grain size within the core decreases. An in-depth analysis of grains and grain boundaries was made to highlight the thermal (such as dynamic recrystallization) or mechanical (such as grains fragmentation by dislocation) contribution within the “core” and “shell.” One of the most widely used methods for determining the dynamic behavior of materials is the SHPB technique developed by Kolsky. A 3D simulation of the SHPB test was created through ABAQUS in dynamic explicit. This 3D simulation allows taking into account all modes of vibration. An inverse approach was used to identify the material parameters from the equation of Johnson-Cook (JC) by minimizing the difference between the numerical and experimental data. The JC’s parameters were identified using B1 and B5 samples configurations. Predictively, identified parameters of JC’s equation shows good result for the other sample configuration. Furthermore, mean rise of temperature within the harmonic Nickel sample can be obtained through ABAQUS and show an elevation of about 35°C for all fives samples. At this temperature, a thermal mechanism cannot be activated. Therefore, grains fragmentation within the core is mainly due to mechanical phenomena for a fixed final strain of 20%.

Keywords: 3D simulation, fragmentation, harmonic structure, high strain rate, Johnson-cook model, microstructure

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Authors: Selam M. Tefera

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Soil constitutes a crucial component of rural and urban environments. This fact is making role of heavy and trace elements in the soil system an issue of global concern. Heavy metals constitute an ill-defined group of inorganic chemical hazards, whose main source is anthropogenic activities mainly related to fabrications. This accumulation of heavy metals soils can prove toxic to the environment. The application of biochar to soil is one way of immobilizing these contaminants through sorption by exploiting the high surface area of this material among its other essential properties. This research examined the ability of sugar cane straw, an organic waste material from sugar farm, derived biochar and ash to remediate soil contaminated with heavy metals mainly Chromium and Zinc from the effluent of electroplating industry. Biochar was produced by varying the temperature from 300 °C to 500 °C and ash at 700 °C. The highest yield (50%) was obtained at the lowest temperature (300 °C). The proximate analysis showed ash content of 42.8%, ultimate analysis with carbon content of 67.18%, the Hydrogen to Carbon ratio of 0.54 and the results from FTIR analysis disclosed the organic nature of biochar. Methylene blue absorption indicated its fine surface area and pore structure, which increases with severity of temperature. Biochar was mixed with soil with at a ration varying from 4% w/w to 10% w/w of soil, and the response variables were determined at a time interval of 150 days, 180 days, and 210 days. As for ash (10% w/w), the characterization was performed at incubation time of 210 days. The results of pH indicated that biochar (9.24) had a notable liming capacity of acidic soil (4.8) by increasing it to 6.89 whereas ash increased it to 7.5. The immobilization capacity of biochar was found to effected mostly by the highest production temperature (500 °C), which was 75.5% for chromium and 80.5% for nickel. In addition, ash was shown to possess an outstanding immobilization capacity of 95.5% and 90.5% for Chromium and Nickel, respectively. All in all, the results from these methods showed that biochar produced from this specific biomass possesses the typical functional groups that enable it to store carbon, the appropriate pH that could remediate acidic soil, a fine amount of macro and micro nutrients that would aid plant growth.

Keywords: biochar, biomass, heavy metal immobalization, soil remediation

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Authors: Z. Kolacinski, L. Szymanski. G. Raniszewski, D. Koza, L. Pietrzak

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Magnetic Bio-Nano-Fluid (BNF) can be composed of a buffer fluid such as plasma and magnetic nanoparticles such as iron, nickel, cobalt and their oxides. However iron is one of the best elements for magnetization by electromagnetic radiation. It can be used as a tool for medical diagnosis and treatment. Radio frequency (RF) radiation is able to heat iron nanoparticles due to magnetic hysteresis. Electromagnetic heating of iron nanoparticles and ferro-fluids BNF can be successfully used for non-invasive thermal ablation of cancer cells. Moreover iron atoms can be carried by carbon nanotubes (CNTs) if iron is used as catalyst for CNTs synthesis. Then CNTs became the iron containers and they screen the iron content against oxidation. We will present a method of CNTs addressing to the required cells. For thermal ablation of cancer cells we use radio frequencies for which the interaction with human body should be limited to minimum. Generally, the application of RF energy fields for medical treatment is justified by deep tissue penetration. The highly iron doped CNTs as the carriers creating magnetic fluid will be presented. An excessive catalyst injection method using electrical furnace and microwave plasma reactor will be presented. This way it is possible to grow the Fe filled CNTs on a moving surface in continuous synthesis process. This also allows producing uniform carpet of the Fe filled CNTs carriers. For the experimental work targeted to cell ablation we used RF generator to measure the increase in temperature for some samples like: solution of Fe2O3 in BNF which can be plasma-like buffer, solutions of pure iron of different concentrations in plasma-like buffer and in buffer used for a cell culture, solutions of carbon nanotubes (MWCNTs) of different concentrations in plasma-like buffer and in buffer used for a cell culture. Then the targeted therapies which can be effective if the carriers are able to distinguish the difference between cancerous and healthy cell’s physiology are considered. We have developed an approach based on ligand-receptor or antibody-antigen interactions for the case of colon cancer.

Keywords: cancer treatment, carbon nano tubes, drag delivery, hyperthermia, iron

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Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

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The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

Procedia PDF Downloads 50

Authors: Salima Agoun-Bahar, Ouzna Abrous-Belbachir, Souad Amelal

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Industrial areas generally contain heavy metals; thus, negative consequences can appear in the medium and long term on the fauna and flora, but also on the food chain, which man constitutes the final link. The SONATRACH Company has become aware of the importance of environmental protection by setting up a rehabilitation program for polluted sites in order to avoid major ecological disasters and find both curative and preventive solutions. The aim of this work consists to study industrial pollution located around a crude oil storage tank in the Algiers refinery of Sidi R'cine and to select the plants which accumulate the most heavy metals for possible use in phytotechnology. Sampling of whole plants with their soil clod was realized around the pollution source at a depth of twenty centimeters, then transported to the laboratory to identify them. The quantification of heavy metals, lead, zinc, copper, and nickel was carried out by atomic absorption spectrophotometry with flame in the soil and at the level of the aerial and underground parts of the plants. Ten plant species were recorded in the polluted site, three of them belonging to the grass family with a dominance percentage higher than 50%, followed by three other species belonging to the Composite family represented by 12% and one species for each of the families Linaceae, Plantaginaceae, Papilionaceae, and Boraginaceae. Koeleria phleoïdes L. and Avena sterilis L. of the grass family seem to be the dominant plants, although they are quite far from the pollution source. Lead pollution of soils is the most pronounced for all stations, with values varying from 237.5 to 2682.5 µg.g⁻¹. Other peaks are observed for zinc (1177 µg.g⁻¹) and copper (635 µg.g⁻¹) at station 8 and nickel (1800 µg.g⁻¹) at station 10. Among the inventoried plants, some species accumulate a significant amount of metals: Trifolium sp and K.phleoides for lead and zinc, P.lanceolata and G.tomentosa for nickel, and A.clavatus for zinc. K.phloides is a very interesting species because it accumulates an important quantity of heavy metals, especially in its aerial part. This can be explained by its use of the phytoextraction technique, which will facilitate the recovery of the pollutants by the simple removal of shoots.

Keywords: heavy metals, industrial pollution, phytotechnology, rehabilitation

Procedia PDF Downloads 39

Authors: Chaima Zoulikha Tabet Zatla, Nihel Dib, Sumeya Bedrane, Juan Carlos Hernandez Garrido, Redouane Bachir, Miguel Angel Cauqui, Jose Juan Calvino Gamez

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These last year's our planet has witnessed global warming, which is a serious threat to our lives; it has many causes, such as the CO₂ excess in the atmosphere that results from our activity, for the purpose of living in a neater and better environment, working and improving an eco-responsible energy system is a must. Valorization of biomass to produce biofuels is among the most compelling routes to decrease air pollution without considerable modification in current vehicle technology. Effective transformation of lignocellulosic biomass-derived compounds into liquid fuels and value-added chemicals is an economically viable solution. Presently, very competitive technics for the conversion of lignocellulosic biomass into platform chemicals, such as furfural and Hydroxymethylfurfural (HMF), are used. Furfural (C₅H₄O₂) is a major hemi cellulosic biomass-derived platform molecule. In our work, we focus on the valorization of lignocellulosic biomass derivative furfural that is transformed into biofuel through a hydrodeoxygenation reaction in general and involving a catalytic process. In order to get to this point, we are synthesizing and characterizing a series of catalysts with different amounts of Ru (0.5%, 1% and 2%) supported on alumina-silica mixed oxides with various molar ratios (Si/Al = 2.5; 5; 7; 10; 15). These catalysts will be characterized by numerous technics such as N₂ adsorption/desorption, Pyridine adsorption (acidity measure), FTIR, X-rays diffraction, AAS, TEM and SEM.

Keywords: furfural, ruthenium, silica-alumina, biomass, biofuel

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Authors: Fadimatou Ngounouno Yamgouota, Isaac Bertrand Gbambié Mbowoub, Ismaila Ngounounob

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Barium and titanium bearing biotite from alkaline trachyte of Upper Benue valley, Northern Cameroon is studied. The iron enrichment index of mica (average I.E.=0.40) is intermediate between annite and phlogopite. The biotite phenocrysts contain up to 6.2 wt. % BaO and 9.8 wt. % TiO2. The BaO content of electron-microprobe mica is positively correlated with the Al2O3, TiO2, and FeO contents, and negatively correlated with the SiO2, K2O, and MgO contents. Ba and Ti rich micas are generally found in in SiO2 deficient rocks, whereas Ba and Ti bearing mica in this study occur in silica-saturated rocks. Most of the phenocrysts analysed have deficiencies in their octahedral and interlayer sites. Deficiencies in the octahedral sites may arise from the Ti vacancy and partly the Ti tschermakite substitution. On the other hand, deficiencies in the interlayer-site are due to the replacement of K by Ba. The substitution mechanism in the Upper Benue valley mica is characterized by Ba + 2Ti + 3Al =(K + Na + Ca) + 3(Mg + Fe + Mn) + 3Si, with an excellent correlation coefficient. Biotite compositions from the Upper Benue valley area fall between the quartz-fayalite-magnetite (QFM) and nickel-nickel-oxide (NNO) oxygen fugacity buffers. All these show that Upper Benue valley mica with high Ba and Ti contents may be formed from magmas rich in these elements.

Keywords: Benue valley, trachyte, biotite, mineral chemistry, enrichment

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Authors: Iftikhar Hussain Gul, Syeda Aatika

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Nickel ferrite was prepared via wet chemical co-precipitation route. Carbon Nano Fibers (CNFs) were used to prepare NiFe₂O₄/CNFs nanohybrids. Polar solvent (ortho-xylene) was used for the dispersion of CNFs in ferrite matrix. X-ray diffraction patterns confirmed the formation of NiFe₂O₄/CNFs nanohybrids without any impurity peak. FTIR patterns showed two consistent characteristic absorption bands for tetrahedral and octahedral sites, confirming the formation of spinel structure of NiFe₂O₄. Scanning Electron Microscopy (SEM) images confirmed the coating of nickel ferrite nanoparticles on CNFs, which confirms the efficiency of deployed method. The dielectric properties were measured as a function of frequency at room temperature. Pure NiFe₂O₄ showed dielectric constant of 1.79 ×10³ at 100 Hz, which increased massively to 2.92 ×10⁶ at 100 Hz with the addition of 20% by weight of CNFs, proving it to be potential candidate for applications in supercapacitors. The impedance analysis showed a considerable decrease of resistance, reactance and cole-cole plot which confirms the decline of impedance on addition of CNFs. The pure NiFe₂O₄ has highest impedance values of 5.89 ×10⁷ Ohm at 100 Hz while the NiFe₂O₄/CNFs nanohybrid with CNFs (20% by weight) has the lowest impedance values of 4.25×10³ Ohm at 100 Hz, which proves this nanohybrid is useful for high-frequency applications.

Keywords: AC impedance, co-precipitation, nanohybrid, Fourier transform infrared spectroscopy, x-ray diffraction

Procedia PDF Downloads 103

Authors: Tesfay Gebremicheal Reda, K. Samatha, Paul Douglas Sanasi, D. Parajuli

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Nanoparticle technology is fast progressing and is being employed in innumerable medical applications. At this time, the public's health is seriously threatened by the rise of bacterial strains resistant to several medications. Metal nanoparticles are a potential alternate approach for tackling this global concern, and this is the main focus of this study. The citrate precursor sol-gel synthesis method was used to synthesize the Niₓ Co₁₋ₓ Fe₂ O₄, (where x = 0.0:0.2:1.0) nanoparticle. XRD identified the development of the cubic crystal structure to have a preferential orientation along (311), and the average particle size was found to be 29-38 nm. The average crystallizes assessed with ImageJ software and origin 22 of the SEM are nearly identical to the XRD results. In the created NCF NPs, the FT-IR spectroscopy reveals structural examinations and the redistribution of cations between octahedral (505-428 cm⁻¹) and tetrahedral (653-603 cm⁻¹) locales. As the Co²⁺ cation is substituted with Ni²⁺, the coercive fields HC decrease from 2384 Oe to 241.93 Oe. Band gap energy rises as Ni concentration increases, which may be attributed to the fact that the ionic radii of Ni²⁺ ions are smaller than that of Co²⁺ ions, which results in a strong electrostatic interaction. On the contrary, except at x = 0.4, the dielectric constant decreases as the nickel concentration increases. According to the findings of this research work, nanoparticles are composed of Ni₀.₄ Co₀.₆ Fe₂ O₄ have demonstrated a promising value against S. aureus and E. coli, and it suggests a proposed model for their potential use as a source of antibacterial agent.

Keywords: antimicrobial, band gap, citrate precursor, dielectric, nanoparticle

Procedia PDF Downloads 26

Authors: Carla Palencia-Aguilar

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In order to attain the 2050’s zero emissions goal, it is necessary to know the carbon dioxide changes over time either from pollution to attenuations in the mining industry versus at green zones to establish real goals and redirect efforts to reduce greenhouse effects. Two methods were used to compute the amount of CO2 tons in specific mining zones in Colombia. The former by means of NPP with MODIS MOD17A3HGF from years 2000 to 2021. The latter by using MODIS MYD021KM bands 33 to 36 with maximum values of 644 data points distributed in 7 sites corresponding to surface mineral mining of: coal, nickel, iron and limestone. The green zones selected were located at the proximities of the studied sites, but further than 1 km to avoid information overlapping. Year 2012 was selected for method 2 to compare the results with data provided by the Colombian government to determine range of values. Some data was compared with 2022 MODIS energy values and converted to kton of CO2 by using the Greenhouse Gas Equivalencies Calculator by EPA. The results showed that Nickel mining was the least pollutant with 81 kton of CO2 e.q on average and maximum of 102 kton of CO2 e.q. per year, with green zones attenuating carbon dioxide in 103 kton of CO2 on average and 125 kton maximum per year in the last 22 years. Following Nickel, there was Coal with average kton of CO2 per year of 152 and maximum of 188, values very similar to the subjacent green zones with average and maximum kton of CO2 of 157 and 190 respectively. Iron had similar results with respect to 3 Limestone sites with average values of 287 kton of CO2 for mining and 310 kton for green zones, and maximum values of 310 kton for iron mining and 356 kton for green zones. One of the limestone sites exceeded the other sites with an average value of 441 kton per year and maximum of 490 kton per year, eventhough it had higher attenuation by green zones than a close Limestore site (3.5 Km apart): 371 kton versus 281 kton on average and maximum 416 kton versus 323 kton, such vegetation contribution is not enough, meaning that manufacturing process should be improved for the most pollutant site. By comparing bands 33 to 36 for years 2012 and 2022 from January to August, it can be seen that on average the kton of CO2 were similar for mining sites and green zones; showing an average yearly balance of carbon dioxide emissions and attenuation. However, efforts on improving manufacturing process are needed to overcome the carbon dioxide effects specially during emissions’ peaks because surrounding vegetation cannot fully attenuate it.

Keywords: carbon dioxide, MODIS, surface mining, vegetation

Procedia PDF Downloads 76

Authors: Nurlan Akhmetov, Abilmansur Yeshmuratov, Aliya Kurbanova, Gulnar Sugurbekova, Murat Baisariyev

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Extraction of the vanadium and nickel compounds is complex due to the high stability of porphyrin, nickel is catalytic poison which deactivates catalysis during the catalytic cracking of the oil, while vanadyl is abrasive and valuable metal. Thus, high concentration of the Ni and V in the crude oil makes their removal relevant. Two methods of the demetallization of crude oil were tested, therefore, the present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits in to the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for Ni and 51.2% for V. Thus, applying the voltammetry, ICP MS (Inductively coupled plasma mass spectrometry) and AAS (atomic absorption spectroscopy), these mentioned types of metal extraction methods were compared in this paper.

Keywords: electrochemistry, deasphalting of crude oil, demetallization of crude oil, petrolium engineering

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Authors: Boukary Lam, Sebastien Deon, Patrick Fievet, Nadia Crini, Gregorio Crini

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Treatment of heavy metal-contaminated industrial wastewater has become a major challenge over the last decades. Conventional processes for the treatment of metal-containing effluents do not always simultaneously satisfy both legislative and economic criteria. In this context, coupling of processes can then be a promising alternative to the conventional approaches used by industry. The polymer-assisted ultrafiltration (PAUF) process is one of these coupling processes. Its principle is based on a sequence of steps with reaction (e.g., complexation) between metal ions and a polymer and a step involving the rejection of the formed species by means of a UF membrane. Unlike free ions, which can cross the UF membrane due to their small size, the polymer/ion species, the size of which is larger than pore size, are rejected. The PAUF process was deeply investigated herein in the case of removal of nickel ions by adding chitosan and carboxymethyl cellulose (CMC). Experiments were conducted with synthetic solutions containing 1 to 100 ppm of nickel ions with or without the presence of NaCl (0.05 to 0.2 M), and an industrial discharge water (containing several metal ions) with and without polymer. Chitosan with a molecular weight of 1.8×105 g mol⁻¹ and a degree of acetylation close to 15% was used. CMC with a degree of substitution of 0.7 and a molecular weight of 9×105 g mol⁻¹ was employed. Filtration experiments were performed under cross-flow conditions with a filtration cell equipped with a polyamide thin film composite flat-sheet membrane (3.5 kDa). Without the step of polymer addition, it was found that nickel rejection decreases from 80 to 0% with increasing metal ion concentration and salt concentration. This behavior agrees qualitatively with the Donnan exclusion principle: the increase in the electrolyte concentration screens the electrostatic interaction between ions and the membrane fixed the charge, which decreases their rejection. It was shown that addition of a sufficient amount of polymer (greater than 10⁻² M of monomer unit) can offset this decrease and allow good metal removal. However, the permeation flux was found to be somewhat reduced due to the increase in osmotic pressure and viscosity. It was also highlighted that the increase in pH (from 3 to 9) has a strong influence on removal performances: the higher pH value, the better removal performance. The two polymers have shown similar performance enhancement at natural pH. However, chitosan has proved more efficient in slightly basic conditions (above its pKa) whereas CMC has demonstrated very weak rejection performances when pH is below its pKa. In terms of metal rejection, chitosan is thus probably the better option for basic or strongly acid (pH < 4) conditions. Nevertheless, CMC should probably be preferred to chitosan in natural conditions (5 < pH < 8) since its impact on the permeation flux is less significant. Finally, ultrafiltration of an industrial discharge water has shown that the increase in metal ion rejection induced by the polymer addition is very low due to the competing phenomenon between the various ions present in the complex mixture.

Keywords: carboxymethyl cellulose, chitosan, heavy metals, nickel ion, polymer-assisted ultrafiltration

Procedia PDF Downloads 131