Search results for: polyvinylidene fluoride (PVDF)

Authors: V. Veena, Suguna Yesodharan, E. P. Yesodharan

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Two Advanced Oxidation Processes (AOP) i.e., sono- and photo-catalysis mediated by semiconductor oxide catalyst, ZnO has been found effective for the removal of trace amounts of the toxic dye pollutant Indigocarmine (IC) from water. The effect of various reaction parameters such as concentration of the dye, catalyst dosage, temperature, pH, dissolved oxygen etc. as well as the addition of oxidisers and presence of salts in water on the rate of degradation has been evaluated and optimised. The degradation follows variable kinetics depending on the concentration of the substrate, the order of reaction varying from 1 to 0 with increase in concentration. The reaction proceeds through a number of intermediates and many of them have been identified using GCMS technique. The intermediates do not affect the rate of degradation significantly. The influence of anions such as chloride, sulphate, fluoride, carbonate, bicarbonate, phosphate etc. on the degradation of IC is not consistent and does not follow any predictable pattern. Phosphates and fluorides inhibit the degradation while chloride, sulphate, carbonate and bicarbonate enhance. Adsorption studies of the dye in the absence as well as presence of these anions show that there may not be any direct correlation between the adsorption of the dye on the catalyst and the degradation. Oxidants such as hydrogen peroxide and persulphate enhance the degradation though the combined effect and it is less than the cumulative effect of individual components. COD measurements show that the degradation proceeds to complete mineralisation. The results will be presented and probable mechanism for the degradation will be discussed.

Keywords: AOP, COD, indigocarmine, photocatalysis, sonocatalysis

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Authors: N. K. A. M. Galvão, A. Godoy Jr., A. L. J. Pereira, G. V. Martins, R. S. Pessoa, H. S. Maciel, M. A. Fraga

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Silicon carbide (SiC) is a wide band-gap semiconductor material with very attractive properties, such as high breakdown voltage, chemical inertness, and high thermal and electrical stability, which makes it a promising candidate for several applications, including microelectromechanical systems (MEMS) and electronic devices. In MEMS manufacturing, the etching process is an important step. It has been proved that wet etching of SiC is not feasible due to its high bond strength and high chemical inertness. In view of this difficulty, the plasma etching technique has been applied with paramount success. However, in most of these studies, only the determination of the etching rate and/or morphological characterization of SiC, as well as the analysis of the reactive ions present in the plasma, are lowly explored. There is a lack of results in the literature on the chemical and structural properties of SiC after the etching process [4]. In this work, we investigated the etching process of sputtered amorphous SiC thin films on Si substrates in a reactive ion etching (RIE) system using sulfur hexafluoride (SF6) gas under different RF power. The results of the chemical and structural analyses of the etched films revealed that, for all conditions, a SiC crystallization occurred, in addition to fluoride contamination. In conclusion, we observed that SiC crystallization is a side effect promoted by structural, morphological and chemical changes caused by RIE SF6 etching process.

Keywords: plasma etching, plasma deposition, Silicon Carbide, microelectromechanical systems

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Authors: Kassahun Tadesse, Megersa O. Dinka

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Drinking water suitability study was conducted for a milky-white stream in remote areas of Ethiopia in order to understand its effect on human health. Water samples were taken from the water source and physicochemical properties were analyzed based on standard methods. The mean values of pH, total dissolved solids, sodium, magnesium, potassium, manganese, chloride, boron, and fluoride were within maximum permissible limits set for health. Whereas turbidity, calcium, irons, hardness, alkalinity, nitrate, and sulfate contents were above the limits. The water is very hard water due to high calcium content. High sulfate content can cause noticeable taste and a laxative (gastrointestinal) effect. The nitrate content was very high and can cause methemoglobinemia (blue baby syndrome) which is a temporary blood disorder in the bottle fed infants. Hence, parents should be advised not to give this water to infants. In conclusion, all physicochemical parameters except for nitrate are safe for health but may affect the appearance and taste, and wear water infrastructures. A high value of turbidity due to suspended minerals is the cause for milky-white colour. However, a mineralogical analysis of suspended sediments is required to identify the exact cause for white colour, and a study on sediment source was recommended.

Keywords: hard water, laxative effect, methemoglobinemia, nitrate, physicochemical, water quality

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Authors: Andrey Norov

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In the recent years, Samoilov Research Institute for Mineral Fertilizers JSC “NIUIF”, the oldest (established in September 1919) industry-oriented institute in Russia, has developed a range of sustainable, environment-friendly, zero-waste technologies that ensure minimal consumption of materials and energy resources and fully consistent with the principles of Green Chemistry that include: - Ecofriendly energy and resource saving technology of sulfuric acid from sulfur according to DC-DA scheme (double conversion - double absorption); - Improved zero-waste technology of wet phosphoric acid (WPA) by dihydrate-hemihydrate process applicable to various types of phosphate raw materials; - Flexible, efficient, zero-waste, universal technology of NP / NPS / NPK / NPKS fertilizers with maximum heat recovery from chemical processes; - Novel, zero-waste, no-analogue technology of granular PK / PKS / NPKS fertilizers with controlled dissolution rate and nutrient supply into the soil, which allows to process a number of wastes and by-products; - Innovative resource-saving joint processing of wastes from the production of phosphogypsum and fluorosilicic acid (FSA) into ammonium sulfate with simultaneous neutralization of fluoride compounds with no lime used. - New fertilizer technology of increased environmental and agrochemical efficiency (currently under development). All listed green technologies are patented with Russian and Eurasian patents. The development of ecofriendly, safe, green technologies is ongoing in JSC “NIUIF”.

Keywords: NPKS fertilizers, FSA, sulfuric acid, WPA

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Authors: Tayyaba Ghani, Mazhar Mehmood, Mohammad Mujahid

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TiO₂ nanotubes are receiving immense attraction in the field of dye-sensitized solar cells due to their well-defined nanostructures, efficient electron transport and large surface area as compared to other one dimensional structures. In the present work, we have investigated the influence of temperature on the morphology of anodically produced self-organized Titanium oxide nanotubes (TiNTs). TiNTs are synthesized by two-step anodization method in an ethylene glycol based electrolytes containing ammonium fluoride. Experiments are performed at constant anodization voltage for two hours. An investigation by the SEM images reveals that if the temperature is kept constant during the anodizing experiment, variation in the average tube diameter is significantly reduced. However, if the temperature is not controlled then due to the exothermic nature of reactions for the formation of TiNTs, the temperature of electrolyte keep on increasing. This variation in electrolyte bath temperature introduced strong variations in tube diameter (20 nm to 160 nm) along the length of tubes. Current profiles, recorded during the anodization experiment, predict the effect of constant and varying experimental temperatures as well. In both cases, XRD results show the complete anatase crystal structure of nanotube upon annealing at 450 °C. Present work highlights the importance of constant temperature during the anodization experiments in order to develop an ordered array of nanotubes with a uniform tube diameter.

Keywords: anodization, ordering, temperature, TiO₂ nanotubes

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Authors: Zainab Abbas Soharwardi, Chunli Su, Fazeelat Tahira, Syed Zahid Aziz

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The study monitors the quality of drinking water consumed by urban population of Lahore. A total of 50 drinking water samples (16 from source and 34 from distribution system) were examined for physical, chemical and bacteriological parameters. The parameters including pH, turbidity, electrical conductivity, total dissolved solids, total hardness, calcium, magnesium, total alkalinity, carbonate, sulphate, chloride, nitrite, fluoride, sodium and potassium were analyzed. Sixteen out of fifty samples showed high values of alkalinity compared to EPA standards and WHO guidelines. Twenty-eight samples were analyzed for heavy metals, chromium, iron, copper, zinc, cadmium and lead. Trace amounts of heavy metals were detected in some samples, however for most of the samples values were within the permissible limits although high concentration of zinc was detected in one sample collected from Mughal Pura area. Fifteen samples were analyzed for arsenic. The results were unsatisfactory; around 73% samples showed exceeding values of As. WHO has suggested permissible limits of arsenic < 0.01 ppm, whereas 27 % of samples have shown 0.05 ppm arsenic, which is five times greater than WHO highest permissible limits. All the samples were examined for E. coli bacteria. On the basis of bacteriological analysis, 42 % samples did not meet WHO guidelines and were unsafe for drinking.

Keywords: arsenic, heavy metals, ground water, Lahore

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Authors: Yongseok Hong, Kurt Louis Solis

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In the present study, a hybrid sorbent using the metal organic framework (MOF), UiO-66, and powdered activated carbon (pAC) is synthesized to remove cationic and anionic metals simultaneously. UiO-66 is an octahedron-shaped MOF with a Zr₆O₄(OH)₄ metal node and 1,4-benzene dicarboxylic acid (BDC) organic linker. Zr-based MOFs are attractive for trace element remediation in wastewaters, because Zr is relatively non-toxic as compared to other classes of MOF and, therefore, it will not cause secondary pollution. Most remediation studies with UiO-66 target anions such as fluoride, but trace element oxyanions such as arsenic, selenium, and antimony have also been investigated. There have also been studies involving mercury removal by UiO-66 derivatives, however these require post-synthetic modifications or have lower effective surface areas. Activated carbon is known for being a readily available, well-studied, effective adsorbent for metal contaminants. Solvothermal method was employed to prepare hybrid sorbent from UiO66 and activated carbon, which could be used to remove mercury and selenium simultaneously. The hybrid sorbent was characterized using FSEM-EDS, FT-IR, XRD, and TGA. The results showed that UiO66 and activated carbon are successfully composited. From BET studies, the hybrid sorbent has a SBET of 1051 m² g⁻¹. Adsorption studies were performed, where the hybrid showed maximum adsorption of 204.63 mg g⁻¹ and 168 mg g⁻¹ for Hg (II) and selenite, respectively, and follows the Langmuir model for both species. Kinetics studies have revealed that the Hg uptake of the hybrid is pseudo-2nd order and has rate constant of 5.6E-05 g mg⁻¹ min⁻¹ and the selenite uptake follows the simplified Elovich model with α = 2.99 mg g⁻¹ min⁻¹, β = 0.032 g mg⁻¹.

Keywords: adsorption, flue gas wastewater, mercury, selenite, metal organic framework

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Authors: Lu-Yin Lin

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The morphology of electroactive material is highly related to energy storage ability. Structure-directing agent (SDA) can design electroactive materials with favorable surface properties. Zeolitic imidazolate framework 67 (ZIF67) is one of the potential electroactive materials for energy storage devices. The SDA concept is less applied to designing ZIF67 derivatives in previous studies. An in-situ technique with ammonium fluoride (NH₄F) as SDA is proposed to produce a ZIF67 derivative with highly improved energy storage ability. Attracted by the effective in-situ technique, the NH₄F, ammonium bifluoride (NH₄HF₂), and ammonium tetrafluoroborate (NH₄BF₄) are first used as SDA to synthesize ZIF67 derivatives in one-step solution process as electroactive material of energy storage devices. The mechanisms of forming ZIF67 derivatives synthesized with different SDAs are discussed to explain the SDA effects on physical and electrochemical properties. The largest specific capacitance (CF) of 1527.0 Fg-¹ and the capacity of 296.9 mAhg-¹ are obtained for the ZIF67 derivative prepared using NH₄BF₄ as SDA. The energy storage device composed of the optimal ZIF67 derivative and carbon electrodes presents a maximum energy density of 15.1 Whkg-¹ at the power density of 857 Wkg-¹. The CF retention of 90% and Coulombic efficiency larger than 98% are also obtained after 5000 cycles.

Keywords: ammonium bifluoride, ammonium tetrafluoroborate, energy storage device, one-step solution process, structure-directing agent, zeolitic imidazolate framework 67

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Authors: Jamil Ahmed, Li P. Wong, Yan P. Chua

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The United Nation's sustainable development goals include the target to ensure access to water and sanitation for all; however, very few studies have assessed school-based drinking water in Pakistan. The purpose of this study was to characterize water quality in primary schools of Pakistan and to characterize how recent WASH interventions were associated with school water quality. We conducted a representative cross-sectional study of primary schools in the Sindh province of Pakistan. We used structured observations and structured interviews to ascertain the school’s WASH conditions. Our primary exposures of interest were the implementation of previous WASH interventions in the school and the water source type. Outcomes of interest included water quality (measured by various chemical and microbiological indicators) and water availability at the school’s primary drinking water source. We used log-binomial regression to characterize how WASH exposures were associated with water quality outcomes. We collected data from 256 schools. Groundwater was the primary drinking water source at most schools (87%). Water testing showed that 14% of the school’s water had arsenic above the WHO recommendations, and over 50% of the water samples exceeded recommendations for both lead and cadmium. A majority of the water sources (52%) had fecal coliform contamination. None of the schools had nitrate contamination (0%), and few had fluoride contamination (5%). Regression results indicated that having a recent WASH intervention at the school was not associated with either arsenic contamination (prevalence ratio=0.97; 95% CI: 0.46-2.1) or with fecal coliform contamination (PR=0.88; 95% CI: 0.67-1.17). Our assessment unveiled several water quality gaps that exist, including high heavy metal and fecal contamination. Our findings will help various stakeholders to take suitable action to improve water quality in Pakistani schools.

Keywords: WASH interventions, water quality, primary school children, heavy metals

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Authors: Yuri A. Kalvachev, Totka D. Todorova

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Zeolite mordenite has been investigated as a transition metal support for the preparation of efficient catalysts in the oxidation of volatile organic compounds (VOCs). The highly crystalline mordenite samples were treated with hydrofluoric acid and ammonium fluoride to get hierarchical material with secondary porosity. The obtained supports by this method have a high active surface area, good diffusion properties and prevent the extraction of metal components during catalytic reactions. The active metal phases platinum and copper were loaded by impregnation on both mordenite materials (parent and acid treated counterparts). Monometalic Pt and Cu, and bimetallic Pt/Cu catalysts were obtained. The metal phases were fine dispersed as nanoparticles on the functional porous materials. The catalysts synthesized in this way were investigated in the reaction of complete oxidation of propane and benzene. Platinum, copper and platinum/copper were loaded and there catalytic activity was investigated and compared. All samples are characterized by X-ray diffraction analysis, nitrogen adsorption, scanning electron microscopy (SEM), X-ray photoelectron measurements (XPS) and temperature programed reduction (TPR). The catalytic activity of the samples obtained is investigated in the reaction of complete oxidation of propane and benzene by using of Gas Chromatography (GC). The oxidation of three organic molecules was investigated—methane, propane and benzene. The activity of metal loaded mordenite catalysts for methane oxidation is almost the same for parent and treated mordenite as a support. For bigger molecules as propane and benzene, the activity of catalysts based on treated mordenite is higher than those based on parent zeolite.

Keywords: metal loaded catalysts, mordenite, VOCs oxidation, zeolites

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Authors: Sandra H. Fukurozaki, Andre L. N. Silva, Joao B. F. Neto, Fernando J. G. Landgraf

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Nowadays, the rare earth (RE) metals play an important role in emerging technologies that are crucial for the decarbonisation of the energy sector. Their unique properties have led to increasing clean energy applications, such as wind turbine generators, and hybrid and electric vehicles. Despite the substantial media coverage that has recently surrounded the mining and processing of rare earth metals, very little quantitative information is available concerning their subsequent life stages, especially related to the metallic production of didymium (Nd-Pr) in fluoride molten salt system. Here we investigate a gate to gate scale life cycle assessment (LCA) of the didymium electrolysis based on three different scenarios of operational conditions. The product system is modeled with SimaPro Analyst 8.0.2 software, and IMPACT 2002+ was applied as an impact assessment tool. In order to develop a life cycle inventories built in software databases, patents, and other published sources together with energy/mass balance were utilized. Analysis indicates that from the 14 midpoint impact categories evaluated, the global warming potential (GWP) is the main contributors to the total environmental burden, ranging from 2.7E2 to 3.2E2 kg CO2eq/kg Nd-Pr. At the damage step assessment, the results suggest that slight changes in materials flows associated with enhancement of current efficiency (between 2.5% and 5%), could lead a reduction up to 12% and 15% of human health and climate change damage, respectively. Additionally, this paper highlights the knowledge gaps and future research efforts needing to understand the environmental impacts of Nd-Pr electrolysis process from the life cycle perspective.

Keywords: didymium electrolysis, environmental impacts, life cycle assessment, rare earth metals

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Authors: Alireza Rafieerad, Bushroa Abd Razak, Bahman Nasiri Tabrizi, Jamunarani Vadivelu

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Recently, reports on the fabrication of nanotubular arrays have generated considerable scientific interest, owing to the broad range of applications of the oxide nanotubes in solar cells, orthopedic and dental implants, photocatalytic devices as well as lithium-ion batteries. A more attractive approach for the fabrication of oxide nanotubes with controllable morphology is the electrochemical anodization of substrate in a fluoride-containing electrolyte. Consequently, titanium dioxide nanotubes (TiO2 NTs) have been highly considered as an applicable material particularly in the district of artificial implants. In addition, regarding long-term efficacy and reasons of failing and infection after surgery of currently used dental implants required to enhance the cytocompatibility properties of Ti-based bone-like tissue. As well, graphene oxide (GO) with relevant biocompatibility features in tissue sites, osseointegration and drug delivery functionalization was fully understood. Besides, the boasting antibacterial ability of silver (Ag) remarkably provided for implantable devices without infection symptoms. Here, surface modification of Ti–6Al–7Nb implants (Ti67IMP) by the development of Ag/GO co-decorated TiO2 NTs was examined. Initially, the anodic TiO2 nanotubes obtained at a constant potential of 60 V were annealed at 600 degree centigrade for 2 h to improve the adhesion of the coating. Afterward, the Ag/GO co-decorated TiO2 NTs were developed by spin coating on Ti67IM. The microstructural features, phase composition and wettability behavior of the nanostructured coating were characterized comparably. In a nutshell, the results of the present study may contribute to the development of the nanostructured Ti67IMP with improved surface properties.

Keywords: anodic tio2 nanotube, biomedical applications, graphene oxide, silver, spin coating

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Authors: Biswajit Pal, Amit Mallik, Anil K. Barik

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Current years have witnessed a phenomenal growth in the research on the rare earth-doped transparent host materials, the essential components in optoelectronics that meet up the increasing demand for fabrication of high quality optical devices especially in telecommunication system. The combination of low phonon energy (because of fluoride environment) and high chemical durability with superior mechanical stability (due to oxide environment) makes the oxyfluoride glass–ceramics the promising and useful materials in optoelectronics. The present work reports on the undoped and doped (1 mol% Pr2O3) glass ceramics of composition 16.52 Al2O3•1.5AlF3• 12.65LaF3•4.33Na2O•64.85 SiO2 (mol%), prepared by melting technique initially that follows annealation at 450 ºC for 1 h. The glass samples so obtained were heat treated at constant 600 ºC with a variation in heat treatment schedule (10- 80 h). TEM techniques were employed to structurally characterize the glass samples. Pr2O3 affects the phase separation in the glass and delays the onset of crystallization in the glass ceramic. The modified crystallization mechanism is established from the analysis of advanced STEM/EDXS results. The phase separated droplets after annealing turn into 10-20 nm of LaF3 nano crystals those upon scrutiny are found to be dotted with the doped Pr3+ ions within the crystals themselves. The EDXS results also suggest that the inner LaF3 crystal core is swallowed by an Al enriched layer that follows a Si enriched surrounding shell as the outer core. This greatly increases the viscosity in the periphery of the crystals that restricts further crystal growth to account for the formation of nano sized crystals.

Keywords: advanced STEM/EDXS, crystallization mechanism, nano crystals, pr3+ ion doped glass and glass ceramic, structural characterization

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Authors: Tabin Millo, Khoob Chand, Ashok Kumar Jaiswal

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Introduction: Various kinds of violence and offences are related to alcohol consumption by the offenders. The relationship between alcohol and violence is complex. But its study is important to achieve understanding of violence as well as alcohol related behavior. This study was done to know the blood alcohol concentration in people involved in various offences and its demographic pattern. The study was carried out in the forensic toxicology laboratory, department of Forensic Medicine, All India Institute of Medical Sciences, New Delhi, India. Material and methods: The blood samples were collected from the arrested people shortly after the commission of the offence by the emergency medical officers in the emergency department and forwarded to the forensic toxicology laboratory through the investigating officer. The blood samples were collected in EDTA vial with sodium fluoride preservative. The samples were analyzed by using gas chromatography with head space (GC-HS), which is ideal for alcohol estimation. The toxicology reports were given within a week. The data of seven years (2011-17) were analyzed for its alcohol concentration, associated crimes and its demographic pattern. Analysis and conclusion: Total 280 samples were analyzed in the period of 2011-2017. All were males except one female who was a bar dancer. The maximum cases were in the age group of 21-30 years (124 cases). The type of offences involved were road traffic accidents (RTA), assault cases, drunken driving, drinking in public place, drunk on duty, sexual offence, bestiality, eve teasing, fall etc. The maximum cases were of assault (75 cases) followed by RTA (64 cases). The maximum cases were in the alcohol concentration range of 101-150mg% (58 cases) followed by 51-100mg% (52 cases). The maximum blood alcohol level detected was 391.51 mg%, belonging to a security guard found unconscious. This study shows that alcohol consumption is associated with various kinds of violence and offences in society.

Keywords: alcohol, crime, toxicology, violence

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Authors: Lee A. Browne, K. Rumbold

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The first fluorinating enzyme, 5'-fluoro-5'-deoxyadenosine synthase (fluorinase) was isolated from the soil bacterium Streptomyces cattleya. Such an enzyme, with the ability to catalyze a C-F bond, presents great potential as a biocatalyst. Naturally fluorinated compounds are extremely rare in nature. As a result, the number of fluorinases identified remains relatively few. The field of fluorination is almost completely synthetic. However, with the increasing demand for fluorinated organic compounds of commercial value in the agrochemical, pharmaceutical and materials industries, it has become necessary to utilize biologically based methods such as biocatalysts. A key step in this crucial process is the large-scale production of the fluorinase enzyme in considerable quantities for industrial applications. Thus, this study aimed to optimize expression of the fluorinase enzyme in both prokaryotic and eukaryotic expression systems in order to obtain high protein yields. The fluorinase gene was cloned into the pET 41b(+) and pPinkα-HC vectors and used to transform the expression hosts, E.coli BL21(DE3) and Pichia pastoris (PichiaPink™ strains) respectively. Expression trials were conducted to select optimal conditions for expression in both expression systems. Fluorinase catalyses a reaction between S-adenosyl-L-Methionine (SAM) and fluoride ion to produce 5'-fluorodeoxyadenosine (5'FDA) and L-Methionine. The activity of the enzyme was determined using HPLC by measuring the product of the reaction 5'FDA. A gradient mobile phase of 95:5 v/v 50mM potassium phosphate buffer to a final mobile phase containing 80:20 v/v 50mM potassium phosphate buffer and acetonitrile were used. This resulted in the complete separation of SAM and 5’-FDA which eluted at 1.3 minutes and 3.4 minutes respectively. This proved that the fluorinase enzyme was active. Optimising expression of the fluorinase enzyme was successful in both E.coli and PichiaPink™ where high expression levels in both expression systems were achieved. Protein production will be scaled up in PichiaPink™ using fermentation to achieve large-scale protein production. High level expression of protein is essential in biocatalysis for the availability of enzymes for industrial applications.

Keywords: biocatalyst, expression, fluorinase, PichiaPink™

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Authors: W. El-Alami, J. Araña, O. González Díaz, J. M. Doña Rodríguez

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The efficiency of the semiconductor TiO₂ needs to be improved to be an effective tool for pollutant removal. To improve the efficiency of this semiconductor, it is necessary to deepen the knowledge of the processes that take place on its surface. In this sense, the deactivation of the catalyst is one of the aspects considered relevant. In order to study this point, the processes of deactivation of TiO₂ during the gas phase degradation of ethanol have been studied. For this, catalysts with only the anatase phase (SA and PC100) and catalysts with anatase and rutile phases (P25 and P90) have been selected. In order to force the deactivation processes, different cycles have been performed, adding ethanol gas but avoiding the degradation of acetates to determine their effect on the process. The surface concentration of fluorine on the catalysts was semi-quantitatively determined by EDAX analysis. The photocatalytic experiments were done with four commercial catalysts (P25, SA, P90, and PC100) and the two fluoride catalysts indicated above. The interaction and photocatalytic degradation of ethanol were followed by Fourier transform infrared spectroscopy (FTIR). EDAX analysis has revealed the presence of sodium on the surface of fluorinated catalysts. In FTIR studies, it has been observed that the acetates adsorbed on the anatase phase in P25 and P90 give rise to electron transfer to surface traps that modify the electronic states of the semiconductor. These deactivation studies have also been carried out with fluorinated P25 and SA catalysts (F-P25 and F-SA) which have observed similar electron transfers but in the opposite direction during illumination. In these materials, it has been observed that the electrons present in the surface traps, as a consequence of the interaction Ti-F, react with the holes, causing a change in the electronic states of the semiconductor. In this way, deactivated states of these materials have been detected by different electron transfer routes. It has been identified that acetates produced from the degradation of ethanol in P25 and P90 are probably hydrated on the surface of the rutile phase. In the catalysts with only the anatase phase (SA and PC100), the deactivation is immediate if the acetates are not removed before adsorbing ethanol again. In F-P25 and F-SA has been observed that the acetates formed react with the sodium ions present on the surface and not with the Ti atoms because they are interacting with the fluorine.

Keywords: photocatalytic degradation, ethanol, TiO₂, deactivation process, F-P25

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Authors: Abhishek N. Srivastava, Rahul Singh, Sumedha Chakma

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The rapid urbanization in the developing countries is generating an enormous amount of waste leading to the creation of unregulated landfill sites at various places at its disposal. The liquid waste, known as leachate, produced from these landfills sites is severely affecting the surrounding water quality. The water quality in the proximity areas of the landfill is found affected by various physico-chemical parameters of leachate such as pH, alkalinity, total hardness, conductivity, chloride, total dissolved solids (TDS), total suspended solids (TSS), sulphate, nitrate, phosphate, fluoride, sodium and potassium, biological parameters such as biochemical oxygen demand (BOD), chemical oxygen demand (COD), Faecal coliform, and heavy metals such as cadmium (Cd), lead (Pb), iron (Fe), mercury (Hg), arsenic (As), cobalt (Co), manganese (Mn), zinc (Zn), copper (Cu), chromium (Cr), nickel (Ni). However, all these parameters are distributive in leachate that produced according to the nature of waste being dumped at various landfill sites, therefore, it becomes very difficult to predict the main responsible parameter of leachate for water quality contamination. The present study is endeavour the comparative analysis of the physical, chemical and biological parameters of various landfills in India viz. Okhla landfill, Ghazipur landfill, Bhalswa ladfill in NCR Delhi, Deonar landfill in Mumbai, Dhapa landfill in Kolkata and Kodungayaiyur landfill, Perungudi landfill in Chennai. The statistical analysis of the parameters was carried out using the Statistical Packages for the Social Sciences (SPSS) and LandSim 2.5 model to simulate the long term effect of various parameters on different time scale. Further, the uncertainties characterization of various input parameters has also been analysed using fuzzy alpha cut (FAC) technique to check the sensitivity of various water quality parameters at the proximity of numerous landfill sites. Finally, the study would help to suggest the best method for the prevention of pollution migration from the landfill sites on priority basis.

Keywords: landfill leachate, water quality, LandSim, fuzzy alpha cut

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Authors: Rim Ben Amor, Myriam Abidi, Moncef Gueddari

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The purpose of the present study is to assess the level and the distribution of CaO, SO3, Cd, Cu, Pb and Zn incore sediments of Ghannouch-Gabes coast, Gulf of Gabes, Tunisian Mediterranean coast. The XRD analyses indicate that the sediments of Ghannouch-Gabes coast are mainly composed of quartz, calcite, gypsum and fluorine reflecting the impact of the phosphate fertilizer industrial waste. The vertical distribution of surface sediments shows for all the elements analyzed, that the area located between the commercial and the fishing port of Gabes, is the most polluted zone, where the two harbors acted as barriers and limited the dispersion of phosphogypsum discharge. The abundance order of metals was found to be Zn > Cd > Cu >Pb and that the highest levels of heavy metals were found in the uppermost segment of the sediment core compared to lower depth subsurface due to a continuous input of PG release and showed that the area between the two harbor suffered from several types of pollutants compared to reference core C1, collected from non-industrialized area. The level of pollution was evaluated using contamination factor (Cf), pollution load index (PLI) and the geoaccumulation index (Igeo). The obtained results of Igeo allowed us to distinguish that the area between the commercial harbor of Ghannouch and the fishing harbor of Gabes is the most polluted where sediments are strongly contaminated for Pb, Cu and Cd. The pollution load index (PLI) of all sediments collected classified them as "polluted". According to contamination factor (Cf), the sediments can be considered as ‘considerable’ to ‘very high’ contaminated for Pb, ‘very high to moderate’ for Cd, ‘ moderate’ for Zn, between ‘moderate’ and ‘considerable’ for Cu. Statistical analyses show that heavy metals, fluoride, calcium and sulphate are resulting from the same anthropogenic origin. The metallic pollution status of sediments of Ghanouch -Gabes coast is worrying and requires a serious intervention.

Keywords: trace metals, phosphogypsum, core sediments, accumulation factor, contamination factor

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Authors: J. Tirano, H. Zea, C. Luhrs

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Photocatalysis has established as viable option in the development of processes for the treatment of pollutants and clean energy production. This option is based on the ability of semiconductors to generate an electron flow by means of the interaction with solar radiation. Owing to its electronic structure, TiO₂ is the most frequently used semiconductors in photocatalysis, although it has a high recombination of photogenerated charges and low solar energy absorption. An alternative to reduce these limitations is the use of nanostructured morphologies which can be produced during the synthesis of TiO₂ nanotubes (TNTs). Therefore, if possible to produce vertically oriented nanostructures it will be possible to generate a greater contact area with electrolyte and better charge transfer. At present, however, the development of these innovative structures still presents an important challenge for the development of competitive photoelectrochemical devices. This research focuses on established correlations between synthesis variables and 1D nanostructure morphology which has a direct effect on the photocatalytic performance. TNTs with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C-550 °C. Morphology and crystalline phase of the TNTs were carried out by SEM, EDS and XRD analysis. As results, the synthesis conditions were established to produce nanostructures with specific morphological characteristics. Anatase was the predominant phase of TNTs after thermal treatment. Nanotubes with 10 μm in length, 40 nm in pore diameter and a surface-volume ratio of 50 are important in photoelectrochemical applications based on TiO₂ due to their 1D characteristics, high surface-volume ratio, reduced radial dimensions and high oxide/electrolyte interface. Finally, this knowledge can be used to improve the photocatalytic activity of TNTs by making additional surface modifications with dopants that improve their efficiency.

Keywords: electrochemical anodization, morphology, self-organized nanotubes, TiO₂ nanotubes

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Authors: Afrouz Yousefi, Mohtada Sadrzadeh

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The widespread presence of poly- and perfluoroalkyl substances (PFAS) poses a significant concern due to their ability to accumulate in living organisms and their persistence in the environment, thanks to their robust carbon-fluorine (C-F) bonds, which require substantial energy to break (485 kJ/mol). The prevalence of toxic PFAS compounds can be highly detrimental to ecosystems, wildlife, and human health. Ongoing efforts are dedicated to investigating methods for fully breaking down and eliminating PFAS from the environment. Among the various techniques employed, advanced oxidation processes have shown promise in completely breaking down emerging contaminants in wastewater. However, the drawback lies in the relatively slow reaction rates of these processes and the substantial energy input required, which currently impedes their widespread commercial adoption. We developed a hybrid process, comprising electro-Fenton as an advanced oxidation process and membrane distillation, to simultaneously degrade organic PFAS pollutants and extract pure water from the mixture. In this study, environmentally persistent perfluorooctanoic acid (PFOA), as an emerging contaminant, was used to study the effectiveness of the electro-Fenton/membrane distillation hybrid system. The PFOA degradation studies were conducted in two modes: electro-Fenton and electro-Fenton coupled with membrane distillation. High-performance liquid chromatography with ultraviolet detection (HPLC-UV), ion-chromatography (measuring fluoride ion concentration), total organic carbon (TOC) decay, mineralization current efficiency (MCE), and specific energy consumption (SEC) were evaluated for a single EF and hybrid EF-MD processes. In contrast to a single EF reaction, TOC decay improved significantly in the EF-MD process. Overall, the MCE of hybrid processes surpassed 100% while it remained under 50% for a single EF reaction. Calculations of specific energy consumption (SEC) demonstrated a substantial decrease of nearly one-third in energy usage when integrating the EF reaction with the MD process.

Keywords: water treatment, PFAS, membrane distillation, electro-Fenton, advanced oxidation

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Authors: V. Golubeva, O. Vakhnina, I. Konopkina, N. Gerasimova, N. Taturina, K. Zhogova

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To improve chemical current sources, the ion-conducting electrolytes based on Li halides (LiCl-KCl, LiCl-LiBr-KBr, LiCl-LiBr-LiF) are developed. It is necessary to have chemical analytical methods for determination of halides to control the electrolytes technology. The methods of classical analytical chemistry are of interest, as they are characterized by high accuracy. Using these methods is a difficult task because halides have similar chemical properties. The objective of this work is to develop a titrimetric method for determining the content of bromides, chlorides, and fluorides in their joint presence in an ion-conducting electrolyte. In accordance with the developed method of analysis to determine fluorides, electrolyte sample is dissolved in diluted HCl acid; fluorides are titrated by La(NO₃)₃ solution with potentiometric indication of equivalence point, fluoride ion-selective electrode is used as sensor. Chlorides and bromides do not form a hardly soluble compound with La and do not interfere in result of analysis. To determine the bromides, the sample is dissolved in a diluted H₂SO₄ acid. The bromides are oxidized with a solution of KIO₃ to Br₂, which is removed from the reaction zone by boiling. Excess of KIO₃ is titrated by iodometric method. The content of bromides is calculated from the amount of KIO₃ spent on Br₂ oxidation. Chlorides and fluorides are not oxidized by KIO₃ and do not interfere in result of analysis. To determine the chlorides, the sample is dissolved in diluted HNO₃ acid and the total content of chlorides and bromides is determined by method of visual mercurometric titration with diphenylcarbazone indicator. Fluorides do not form a hardly soluble compound with mercury and do not interfere with determination. The content of chlorides is calculated taking into account the content of bromides in the sample of electrolyte. The validation of the developed analytical method was evaluated by analyzing internal reference material with known chlorides, bromides and fluorides content. The analytical method allows to determine chlorides, bromides and fluorides in case of their joint presence in ion-conducting electrolyte within the range and with relative total error (δ): for bromides from 60.0 to 65.0 %, δ = ± 2.1 %; for chlorides from 8.0 to 15.0 %, δ = ± 3.6 %; for fluorides from 5.0 to 8.0%, ± 1.5% . The analytical method allows to analyze electrolytes and mixtures that contain chlorides, bromides, fluorides of alkali metals and their mixtures (K, Na, Li).

Keywords: bromides, chlorides, fluorides, ion-conducting electrolyte

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Authors: Qing Liu, Jean-fabien Capsal, Claude Richard

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In this current contribution, authors are dedicated to investigate influence of the crystal lamellae orientation on electromechanical behaviors of relaxor ferroelectric Poly (vinylidene fluoride –trifluoroethylene -chlorotrifluoroethylene) (P(VDF-TrFE-CTFE)) films by control of polymer microstructure, aiming to picture the full map of structure-property relationship. In order to define their crystal orientation films, terpolymer films were fabricated by solution-casting, stretching and hot-pressing process. Differential scanning calorimetry, impedance analyzer, and tensile strength techniques were employed to characterize crystallographic parameters, dielectric permittivity, and elastic Young’s modulus respectively. In addition, large electrical induced out-of-plane electrostrictive strain was obtained by cantilever beam mode. Consequently, as-casted pristine films exhibited surprisingly high electrostrictive strain 0.1774% due to considerably small value of elastic Young’s modulus although relatively low dielectric permittivity. Such reasons contributed to large mechanical elastic energy density. Instead, due to 2 folds increase of elastic Young’s modulus and less than 50% augmentation of dielectric constant, fully-crystallized film showed weak electrostrictive behavior and mechanical energy density as well. And subjected to mechanical stretching process, Film C exhibited stronger dielectric constant and out-performed electrostrictive strain over Film B because edge-on crystal lamellae orientation induced by uniaxially mechanical stretch. Hot-press films were compared in term of cooling rate. Rather large electrostrictive strain of 0.2788% for hot-pressed Film D in quenching process was observed although its dielectric permittivity equivalent to that of pristine as-casted Film A, showing highest mechanical elastic energy density value of 359.5 J/m^3. In hot-press cooling process, dielectric permittivity of Film E saw values at 48.8 concomitant with ca.100% increase of Young’s modulus. Films with intermediate mechanical energy density were obtained.

Keywords: crystal orientation, electrostroctive strain, mechanical energy density, permittivity, relaxor ferroelectric

Procedia PDF Downloads 346

Authors: Kei Kamada, Rikito Murakami, Masahiko Ito, Mototaka Arakawa, Yasuhiro Shoji, Toshiyuki Ueno, Masao Yoshino, Akihiro Yamaji, Shunsuke Kurosawa, Yuui Yokota, Yuji Ohashi, Akira Yoshikawa

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Techniques of energy harvesting y have been widely developed in recent years, due to high demand on the power supply for ‘Internet of things’ devices such as wireless sensor nodes. In these applications, conversion technique of mechanical vibration energy into electrical energy using magnetostrictive materials n have been brought to attention. Among the magnetostrictive materials, Fe-Ga and Fe-Al alloys are attractive materials due to the figure of merits such price, mechanical strength, high magnetostrictive constant. Up to now, bulk crystals of these alloys are produced by the Bridgman–Stockbarger method or the Czochralski method. Using these method big bulk crystal up to 2~3 inch diameter can be grown. However, non-uniformity of chemical composition along to the crystal growth direction cannot be avoid, which results in non-uniformity of magnetostriction constant and reduction of the production yield. The micro-pulling down (μ-PD) method has been developed as a shaped crystal growth technique. Our group have reported shaped crystal growth of oxide, fluoride single crystals with different shape such rod, plate tube, thin fiber, etc. Advantages of this method is low segregation due to high growth rate and small diffusion of melt at the solid-liquid interface, and small kerf loss due to near net shape crystal. In this presentation, we report the shaped long plate crystal growth of Fe-Ga and Fe-Al alloys using the μ-PD method. Alloy crystals were grown by the μ-PD method using calcium oxide crucible and induction heating system under the nitrogen atmosphere. The bottom hole of crucibles was 5 x 1mm² size. A <100> oriented iron-based alloy was used as a seed crystal. 5 x 1 x 320 mm³ alloy crystal plates were successfully grown. The results of crystal growth, chemical composition analysis, magnetostrictive properties and a prototype vibration energy harvester are reported. Furthermore, continuous crystal growth using powder supply system will be reported to minimize the chemical composition non-uniformity along the growth direction.

Keywords: crystal growth, micro-pulling-down method, Fe-Ga, Fe-Al

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Authors: Boriana Karamanova, Svetlana Veleva, Luybomir Soserov, Ana Arenillas, Francesco Lufrano, Antonia Stoyanova

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Supercapacitors have received a lot of research attention and are promising energy storage devices due to their high power and long cycle life. In order to developed an advanced device with significant capacity for storing charge and cheap carbon materials, efforts must focus not only on improving synthesis by controlling the morphology and pore size but also on improving electrode-electrolyte compatibility of the resulting systems. The present study examines the relationship between the surface chemistry of two activated carbon xerogels, the electrolyte type, and the electrochemical properties of supercapacitors. Activated carbon xerogels were prepared by varying the initial pH of the resorcinol-formaldehyde aqueous solution. The materials produced are physicochemical characterized by DTA/TGA, porous characterization, and SEM analysis. The carbon xerogel based electrodes were prepared by spreading over glass plate a slurry containing the carbon gel, graphite, and poly vinylidene difluoride (PVDF) binder. The layer formed was dried consecutively at different temperatures and then detached by water. After, the layer was dried again to improve its mechanical stability. The developed electrode materials and the Aquivion® E87-05S membrane (Solvay Specialty Polymers), socked in Na2SO4 as a polymer electrolyte, were used to assembly the solid-state supercapacitor. Symmetric supercapacitor cells composed by same electrodes and 1 M KOH electrolytes are also assembled and tested for comparison. The supercapacitor performances are verified by different electrochemical methods - cyclic voltammetry, galvanostatic charge/discharge measurements, electrochemical impedance spectroscopy, and long-term durability tests in neutral and alkaline electrolytes. Specific capacitances, energy, and power density, energy efficiencies, and durability were compared into studied supercapacitors. Ex-situ physicochemical analyses on the synthesized materials have also been performed, which provide information about chemical and structural changes in the electrode morphology during charge / discharge durability tests. They are discussed on the basis of electrode-electrolyte interaction. The obtained correlations could be of significance in order to design sustainable solid-state supercapacitors with high power and energy density. Acknowledgement: This research is funded by the Ministry of Education and Science of Bulgaria under the National Program "European Scientific Networks" (Agreement D01-286 / 07.10.2020, D01-78/30.03.2021). Authors gratefully acknowledge.

Keywords: carbon xerogel, electrochemical tests, neutral and alkaline electrolytes, supercapacitors

Procedia PDF Downloads 103

Authors: Hilal Köse, Şeyma Dombaycıoğlu, Ali Osman Aydın, Hatem Akbulut

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Rechargeable lithium-ion batteries (LIBs) have become promising power sources for a wide range of applications, such as mobile communication devices, portable electronic devices and electrical/hybrid vehicles due to their long cycle life, high voltage and high energy density. Graphite, as anode material, has been widely used owing to its extraordinary electronic transport properties, large surface area, and high electrocatalytic activities although its limited specific capacity (372 mAh g-1) cannot fulfil the increasing demand for lithium-ion batteries with higher energy density. To settle this problem, many studies have been taken into consideration to investigate new electrode materials and metal oxide/graphene composites are selected as a kind of promising material for lithium ion batteries as their specific capacities are much higher than graphene. Among them, SnO₂, an n-type and wide band gap semiconductor, has attracted much attention as an anode material for the new-generation lithium-ion batteries with its high theoretical capacity (790 mAh g-1). However, it suffers from large volume changes and agglomeration associated with the Li-ion insertion and extraction processes, which brings about failure and loss of electrical contact of the anode. In addition, there is also a huge irreversible capacity during the first cycle due to the formation of amorphous Li₂O matrix. To obtain high capacity anode materials, we studied on the synthesis and characterization of SnO₂-Graphene nanocomposites and investigated the capacity of this free-standing anode material in this work. For this aim, firstly, graphite oxide was obtained from graphite powder using the method described by Hummers method. To prepare the nanocomposites as free-standing anode, graphite oxide particles were ultrasonicated in distilled water with SnO2 nanoparticles (1:1, w/w). After vacuum filtration, the GO-SnO₂ paper was peeled off from the PVDF membrane to obtain a flexible, free-standing GO paper. Then, GO structure was reduced in hydrazine solution. Produced SnO2- graphene nanocomposites were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), and X-ray diffraction (XRD) analyses. CR2016 cells were assembled in a glove box (MBraun-Labstar). The cells were charged and discharged at 25°C between fixed voltage limits (2.5 V to 0.2 V) at a constant current density on a BST8-MA MTI model battery tester with 0.2C charge-discharge rate. Cyclic voltammetry (CV) was performed at the scan rate of 0.1 mVs-1 and electrochemical impedance spectroscopy (EIS) measurements were carried out using Gamry Instrument applying a sine wave of 10 mV amplitude over a frequency range of 1000 kHz-0.01 Hz.

Keywords: SnO₂-graphene, nanocomposite, anode, Li-ion battery

Procedia PDF Downloads 199

Authors: J. Tirano, H. Zea, C. Luhrs

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It is well known that titanium dioxide is a semiconductor with several applications in photocatalytic process. Its band gap makes it very interesting in the photoelectrodes manufacturing used in photoelectrochemical cells for hydrogen production, a clean and environmentally friendly fuel. The synthesis of 1D titanium dioxide nanostructures, such as nanotubes, makes possible to produce more efficient photoelectrodes for solar energy to hydrogen conversion. In essence, this is because it increases the charge transport rate, decreasing recombination options. However, its principal constraint is to be mainly sensitive to UV range, which represents a very low percentage of solar radiation that reaches earth's surface. One of the alternatives to modifying the TiO2’s band gap and improving its photoactivity under visible light irradiation is to dope the nanotubes with transition metals. This option requires fabricating efficient nanostructured photoelectrodes with controlled morphology and specific properties able to offer a suitable surface area for metallic doping. Hence, currently one of the central challenges in photoelectrochemical cells is the construction of nanomaterials with a proper band position for driving the reaction while absorbing energy over the VIS spectrum. This research focuses on the synthesis and characterization of Nidoped TiO2 nanotubes for improving its photocatalytic activity in solar energy conversion applications. Initially, titanium dioxide nanotubes (TNTs) with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C - 550 °C. Afterwards, the nanotubes were superficially modified by nickel deposition. Morphology and crystalline phase of the samples were carried out by SEM, EDS and XRD analysis before and after nickel deposition. Determining the photoelectrochemical performance of photoelectrodes is based on typical electrochemical characterization techniques. Also, the morphological characterization associated electrochemical behavior analysis were discussed to establish the effect of nickel nanoparticles modification on the TiO2 nanotubes. The methodology proposed in this research allows using other transition metal for nanotube surface modification.

Keywords: dimensionally stable electrode, nickel nanoparticles, photo-electrode, TiO₂ nanotubes

Procedia PDF Downloads 151

Authors: S. M. D. Y. S. A. Wijayarathna, A. C. A. Jayasundera

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Mahaweli River is the longest and largest river in Sri Lanka and it is the major drinking water source for a large portion of 2.5 million inhabitants in the Central Province. The aim of this study was to the determination of water quality and aquatic life health quality in a selected region of Mahaweli River. Six sampling locations (Site 1: 7° 16' 50" N, 80° 40' 00" E; Site 2: 7° 16' 34" N, 80° 40' 27" E; Site 3: 7° 16' 15" N, 80° 41' 28" E; Site 4: 7° 14' 06" N, 80° 44' 36" E; Site 5: 7° 14' 18" N, 80° 44' 39" E; Site 6: 7° 13' 32" N, 80° 46' 11" E) with various anthropogenic activities at bank of the river were selected for a period of three months from Tennekumbura Bridge to Victoria Reservoir. Temperature, pH, Electrical Conductivity (EC), Total Dissolved Solids (TDS), Dissolved Oxygen (DO), 5-day Biological Oxygen Demand (BOD5), Total Suspended Solids (TSS), hardness, the concentration of anions, and metal concentration were measured according to the standard methods, as physicochemical parameters. Planktons were considered as biological parameters. Using a plankton net (20 µm mesh size), surface water samples were collected into acid washed dried vials and were stored in an ice box during transportation. Diversity and abundance of planktons were identified within 4 days of sample collection using standard manuals of plankton identification under the light microscope. Almost all the measured physicochemical parameters were within the CEA standards limits for aquatic life, Sri Lanka Standards (SLS) or World Health Organization’s Guideline for drinking water. Concentration of orthophosphate ranged between 0.232 to 0.708 mg L-1, and it has exceeded the standard limit of aquatic life according to CEA guidelines (0.400 mg L-1) at Site 1 and Site 2, where there is high disturbance by cultivations and close households. According to the Pearson correlation (significant correlation at p < 0.05), it is obvious that some physicochemical parameters (temperature, DO, TDS, TSS, phosphate, sulphate, chloride fluoride, and sodium) were significantly correlated to the distribution of some plankton species such as Aulocoseira, Navicula, Synedra, Pediastrum, Fragilaria, Selenastrum, Oscillataria, Tribonema and Microcystis. Furthermore, species that appear in blooms (Aulocoseira), organic pollutants (Navicula), and phosphate high eutrophic water (Microcystis) were found, indicating deteriorated water quality in Mahaweli River due to agricultural activities, solid waste disposal, and release of domestic effluents. Therefore, it is necessary to improve environmental monitoring and management to control the further deterioration of water quality of the river.

Keywords: bio indicator, environmental variables, planktons, physicochemical parameters, water quality

Procedia PDF Downloads 79

Authors: Alice Robba, Renaud Bouchet, Celine Barchasz, Jean-Francois Colin, Erik Elkaim, Kristina Kvashnina, Gavin Vaughan, Matjaz Kavcic, Fannie Alloin

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With their high theoretical energy density (~2600 Wh.kg-1), lithium/sulfur (Li/S) batteries are highly promising, but these systems are still poorly understood due to the complex mechanisms/equilibria involved. Replacing S8 by Li2S as the active material allows the use of safer negative electrodes, like silicon, instead of lithium metal. S8 and Li2S have different conductivity and solubility properties, resulting in a profoundly changed activation process during the first cycle. Particularly, during the first charge a high polarization and a lack of reproducibility between tests are observed. Differences observed between raw Li2S material (micron-sized) and that electrochemically produced in a battery (nano-sized) may indicate that the electrochemical process depends on the particle size. Then the major focus of the presented work is to deepen the understanding of the Li2S material charge mechanism, and more precisely to characterize the effect of the initial Li2S particle size both on the mechanism and the electrode preparation process. To do so, Li2S nanoparticles were synthetized according to two ways: a liquid path synthesis and a dissolution in ethanol, allowing Li2S nanoparticles/carbon composites to be made. Preliminary chemical and electrochemical tests show that starting with Li2S nanoparticles could effectively suppress the high initial polarization but also influence the electrode slurry preparation. Indeed, it has been shown that classical formulation process - a slurry composed of Polyvinylidone Fluoride polymer dissolved in N-methyle-2-pyrrolidone - cannot be used with Li2S nanoparticles. This reveals a complete different Li2S material behavior regarding polymers and organic solvents when going at the nanometric scale. Then the coupling between two operando characterizations such as X-Ray Diffraction (XRD) and X-Ray Absorption and Emission Spectroscopy (XAS/XES) have been carried out in order to interpret the poorly understood first charge. This study discloses that initial particle size of the active material has a great impact on the working mechanism and particularly on the different equilibria involved during the first charge of the Li2S based Li-ion batteries. These results explain the electrochemical differences and particularly the polarization differences observed during the first charge between micrometric and nanometric Li2S-based electrodes. Finally, this work could lead to a better active material design and so to more efficient Li2S-based batteries.

Keywords: Li-ion/Sulfur batteries, Li2S nanoparticles effect, Operando characterizations, working mechanism

Procedia PDF Downloads 237

Authors: Tim Bolle, Franziska Kreimendahl, Thomas Gries, Stefan Jockenhoevel

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The therapeutic treatment of extensive, deep wounds is limited. Autologous split-skin grafts are used as a so-called ‘gold standard’. Most common deficits are the defects at the donor site, the risk of scarring as well as the limited availability and quality of the autologous grafts. The aim of this project is a tissue engineered dermal-epidermal skin replacement to overcome the limitations of the gold standard. A key requirement for the development of such a three-dimensional implant is the formation of a functional capillary-like network inside the implant to ensure a sufficient nutrient and gas supply. Tailored three-dimensional warp knitted spacer fabrics are used to reinforce the mechanically week fibrin gel-based scaffold and further to create a directed in vitro pre-vascularization along the parallel-oriented pile yarns within a co-culture. In this study various three-dimensional warp knitted spacer fabrics were developed in a factorial design to analyze the influence of the machine parameters such as the stitch density and the pattern of the fabric on the scaffold performance and further to determine suitable parameters for a successful fibrin gel-incorporation and a physiological performance of the scaffold. The fabrics were manufactured on a Karl Mayer double-bar raschel machine DR 16 EEC/EAC. A fine machine gauge of E30 was used to ensure a high pile yarn density for sufficient nutrient, gas and waste exchange. In order to ensure a high mechanical stability of the graft, the fabrics were made of biocompatible PVDF yarns. Key parameters such as the pore size, porosity and stress/strain behavior were investigated under standardized, controlled climate conditions. The influence of the input parameters on the mechanical and morphological properties as well as the ability of fibrin gel incorporation into the spacer fabric was analyzed. Subsequently, the pile yarns of the spacer fabrics were colonized with Human Umbilical Vein Endothelial Cells (HUVEC) to analyze the ability of the fabric to further function as a guiding structure for a directed vascularization. The cells were stained with DAPI and investigated using fluorescence microscopy. The analysis revealed that the stitch density and the binding pattern have a strong influence on both the mechanical and morphological properties of the fabric. As expected, the incorporation of the fibrin gel was significantly improved with higher pore sizes and porosities, whereas the mechanical strength decreases. Furthermore, the colonization trials revealed a high cell distribution and density on the pile yarns of the spacer fabrics. For a tailored reinforcing structure, the minimum porosity and pore size needs to be evaluated which still ensures a complete incorporation of the reinforcing structure into the fibrin gel matrix. That will enable a mechanically stable dermal graft with a dense vascular network for a sufficient nutrient and oxygen supply of the cells. The results are promising for subsequent research in the field of reinforcing mechanically weak biological scaffolds and develop functional three-dimensional scaffolds with an oriented pre-vascularization.

Keywords: fibrin-gel, skin replacement, spacer fabric, pre-vascularization

Procedia PDF Downloads 230

Authors: Aipeng Zhu, Yun Zhang

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The growing grievous environment problems together with the exhaustion of energy resources put urgent demands for developing high energy density. Considering the factors including capacity, resource and environment, Manganese-based lithium-rich layer-structured cathode materials xLi₂MnO₃⋅(1-x)LiMO₂ (M = Ni, Co, Mn, and other metals) are drawing increasing attention due to their high reversible capacities, high discharge potentials, and low cost. They are expected to be one type of the most promising cathode materials for the next-generation Li-ion batteries (LIBs) with higher energy densities. Unfortunately, their commercial applications are hindered with crucial drawbacks such as poor rate performance, limited cycle life and continuous falling of the discharge potential. With decades of extensive studies, significant achievements have been obtained in improving their cyclability and rate performances, but they cannot meet the requirement of commercial utilization till now. One major problem for lithium-rich layer-structured cathode materials (LLOs) is the side reaction during cycling, which leads to severe surface degradation. In this process, the metal ions can dissolve in the electrolyte, and the surface phase change can hinder the intercalation/deintercalation of Li ions and resulting in low capacity retention and low working voltage. To optimize the LLOs cathode material, the surface coating is an efficient method. Considering the price and stability, Al₂O₃ was used as a coating material in the research. Meanwhile, due to the low initial Coulombic efficiency (ICE), the pristine LLOs was pretreated by KMnO₄ to increase the ICE. The precursor was prepared by a facile coprecipitation method. The as-prepared precursor was then thoroughly mixed with Li₂CO₃ and calcined in air at 500℃ for 5h and 900℃ for 12h to produce Li₁.₂[Ni₀.₂Mn₀.₆]O₂ (LNMO). The LNMO was then put into 0.1ml/g KMnO₄ solution stirring for 3h. The resultant was filtered and washed with water, and dried in an oven. The LLOs obtained was dispersed in Al(NO₃)₃ solution. The mixture was lyophilized to confer the Al(NO₃)₃ was uniformly coated on LLOs. After lyophilization, the LLOs was calcined at 500℃ for 3h to obtain LNMO@LMO@ALO. The working electrodes were prepared by casting the mixture of active material, acetylene black, and binder (polyvinglidene fluoride) dissolved in N-methyl-2-pyrrolidone with a mass ratio of 80: 15: 5 onto an aluminum foil. The electrochemical performance tests showed that the multiple surface modified materials had a higher initial Coulombic efficiency (84%) and better capacity retention (91% after 100 cycles) compared with that of pristine LNMO (76% and 80%, respectively). The modified material suggests that the KMnO₄ pretreat and Al₂O₃ coating can increase the ICE and cycling stability.

Keywords: Li-rich materials, surface coating, lithium ion batteries, Al₂O₃

Procedia PDF Downloads 104