Search results for: nano-sized

Authors: Jenny Radeva, Anke-Gundula Roth, Christian Goebbert, Robert Niestroj-Pahl, Lars Daehne, Axel Wolfram, Juergen Wiese

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The technological advantages of ceramic filtration elements were combined with polyelectrolyte films in the development process of hybrid membrane for the elimination of pharmaceuticals from Aquarius solutions. Previously extruded alumina ceramic membranes were coated with nanosized polyelectrolyte films using Layer-by-Layer technology. The polyelectrolyte chains form a network with nano-pores on the ceramic surface and promote the retention of small molecules like pharmaceuticals and microplastics, which cannot be eliminated using standard ultrafiltration methods. Additionally, the polyelectrolyte coat contributes with its adjustable (based on application) Zeta Potential for repulsion of contaminant molecules with opposite charges. Properties like permeability, bubble point, pore size distribution and Zeta Potential of ceramic and hybrid membranes were characterized using various laboratory and pilot tests and compared with each other. The most significant role for the membrane characterization played the filtration behavior investigation, during which retention against widely used pharmaceuticals like Diclofenac, Ibuprofen and Sulfamethoxazol was subjected to series of filtration tests. The presented study offers a new perspective on nanosized molecules removal from aqueous solutions and shows the importance of combined techniques application for the elimination of pharmaceutical contaminants from drinking water.

Keywords: water treatment, hybrid membranes, layer-by-layer coating, filtration, polyelectrolytes

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Authors: A. Katsman, L. Bloch, Y. Etinger, Y. Kauffmann, B. Pokroy

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Various nanosized amorphous alumina thin films in the range of (2.4 - 63.1) nm were deposited onto amorphous carbon and amorphous Si3N4 membrane grids. Transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), X-ray photoelectron spectroscopy (XPS) and differential scanning calorimetry (DSC) techniques were used to probe the size effect on the short range order and the amorphous to crystalline phase transition temperature. It was found that the short-range order changes as a function of size: the fraction of tetrahedral Al sites is greater in thinner amorphous films. This result correlates with the change of amorphous alumina density with the film thickness demonstrated by the reflectivity experiments: the thinner amorphous films have the less density. These effects are discussed in terms of surface reconstruction of the amorphous alumina films. The average atomic binding energy in the thin film layer decreases with decease of the thickness, while the average O-Al interatomic distance increases. The reconstruction of amorphous alumina is induced by the surface reconstruction, and the short range order changes being dependent on the density. Decrease of the surface energy during reconstruction is the driving force of the alumina reconstruction (density change) followed by relaxation process (short range order change). The amorphous to crystalline phase transition temperature measured by DSC rises with the decrease in thickness from 997.6°C for 13.9 nm to 1020.4 °C for 2.7 nm thick. This effect was attributed to the different film densities: formation of nanovoids preceding and accompanying crystallization process influences the crystallization rate, and by these means, the temperature of crystallization peak.

Keywords: amorphous alumina, density, short range order, size effect

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Authors: K. Tomolya, D. Janovszky, A. Sycheva, M. Sveda, A. Roosz

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CuZrAl amorphous alloys have attracted high interest due to unique physical and mechanical properties, which can be enhanced by adding of Ni and Ti elements. It is known that this properties can be enhanced by crystallization of amorphous alloys creating nanocrystallines in the matrix. The present work intends to produce nanosized crystalline parti-cle reinforced amorphous matrix composite powders by crystallization of amorphous powders. As the first step the amorphous powders were synthe-tized by ball-milling of crystalline powders. (Cu49Zr45Al6) 80Ni10Ti10 and (Cu49Zr44Al7) 80Ni10Ti10 (at%) alloys were ball-milled for 12 hours in order to reach the fully amorphous structure. The impact en-ergy of the balls during milling causes the change of the structure in the powders. Scanning electron microscopical (SEM) images shows that the phases mixed first and then changed into a fully amorphous matrix. Furthermore, nanosized particles in the amorphous matrix were crystallized by heat treatment of the amorphous powders that was confirmed by TEM measurement. It was of importance to define the tem-perature when the amorphous phase starts to crystal-lize. Amorphous alloys have a special heating curve and characteristic temperatures, which can be meas-ured by differential scanning calorimetry (DSC). A typical DSC curve of an amorphous alloy exhibits an endothermic event characteristic of the equilibrium glass transition (Tg) and a distinct undercooled liquid region, followed by one or two exothermic events corresponding to crystallization processes (Tp). After measuring the DSC traces of the amorphous powders, the annealing temperatures should be determined between Tx and Tp. In our experiments several temperatures from the annealing temperature range were selected and de-pendency of crystallized nanoparticles fraction on their hardness was investigated.

Keywords: amorphous structure, composite, mechanical milling, powder, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electronmocroscopy (TEM)

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Authors: Laura Elena De León Prado, Dora Alicia Cortés Hernández, Javier Sánchez

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Among the different cancer treatments that are currently used, hyperthermia has a promising potential due to the multiple benefits that are obtained by this technique. In general terms, hyperthermia is a method that takes advantage of the sensitivity of cancer cells to heat, in order to damage or destroy them. Within the different ways of supplying heat to cancer cells and achieve their destruction or damage, the use of magnetic nanoparticles has attracted attention due to the capability of these particles to generate heat under the influence of an external magnetic field. In addition, these nanoparticles have a high surface area and sizes similar or even lower than biological entities, which allow their approaching and interaction with a specific region of interest. The most used magnetic nanoparticles for hyperthermia treatment are those based on iron oxides, mainly magnetite and maghemite, due to their biocompatibility, good magnetic properties and chemical stability. However, in order to fulfill more efficiently the requirements that demand the treatment of magnetic hyperthermia, there have been investigations using ferrites that incorporate different metallic ions, such as Mg, Mn, Co, Ca, Ni, Cu, Li, Gd, etc., in their structure. This paper reports the synthesis of nanosized Mg_xMn_1-xFe₂O₄ (x = 0.3 and 0.4) ferrites by sol-gel method and their evaluation in terms of heating capability and in vitro hemolysis to determine the potential use of these nanoparticles as thermoseeds for the treatment of cancer by magnetic hyperthermia. It was possible to obtain ferrites with nanometric sizes, a single crystalline phase with an inverse spinel structure and a behavior near to that of superparamagnetic materials. Additionally, at concentrations of 10 mg of magnetic material per mL of water, it was possible to reach a temperature of approximately 45°C, which is within the range of temperatures used for the treatment of hyperthermia. The results of the in vitro hemolysis assay showed that, at the concentrations tested, these nanoparticles are non-hemolytic, as their percentage of hemolysis is close to zero. Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia.

Keywords: ferrites, heating capability, hemolysis, nanoparticles, sol-gel

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Authors: Ahmad Umar, Ahmed A. Ibrahim, Mohsen A. Alhamami

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This study introduces a facile synthesis method for synthesizing reduced graphene oxide (rGO) nanosheets with surface decoration of polyaniline (PANI). The resultant rGO@PANI nanocomposite (NC) exhibit substantial potential as advanced electrode materials for high-performance supercapacitors. The strategic integration of PANI onto the rGO surface serves dual purposes, effectively mitigating the agglomeration of rGO films and augmenting their utility in supercapacitor applications. The PANI coating manifests a highly porous and nanosized morphology, fostering increased surface area and optimized mass transport by reducing diffusion kinetics. The nanosized structure of PANI contributes to the maximization of active sites, thereby bolstering the efficacy of the nanocomposites for diverse applications. The inherent conductive nature of the rGO surface significantly expedites electron transport, thereby amplifying the overall electrochemical performance of the nanocomposites. To systematically evaluate the influence of PANI concentration on the electrode performance, varying concentrations of PANI were incorporated. Notably, an elevated PANI concentration was found to enhance the response owing to the unique morphology of PANI. Remarkably, the 5% rGO@PANI NC emerged as the most promising candidate, demonstrating exceptional response characteristics with a specific capacitance of 314.2 F/g at a current density of 1 A/g. Furthermore, this catalyst exhibits outstanding long-term stability, retaining approximately 92% of its capacitance even after enduring 4000 cycles. This research underscores the significance of the synergistic integration of rGO and PANI in the design of high-performance supercapacitors. The elucidation of the underlying mechanisms governing the improved electrochemical properties contributes to the fundamental understanding of nanocomposite behavior, thereby paving the way for the rational design of next-generation energy storage materials.

Keywords: reduced graphene oxide, polyaniline, nanocomposites, supercapacitors, energy storage

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Authors: Krasimir Ivanov, Elitsa Kolentsova, Nguyen Nguyen, Alexander Peltekov, Violina Angelova

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The nanosized zinc hydroxide nitrate has been recently estimated as perspective foliar fertilizer, which has improved zinc solubility, but low phytotoxicity, in comparison with ZnO and other Zn containing compounds. The main problem is obtaining of stable particles with dimensions less than 100 nm. This work studies the effect of preparation conditions on the chemical compositions and particle size of the zinc hydroxide nitrates, prepared by precipitation. Zn(NO3)2.6H2O and NaOH with concentrations, ranged from 0.2 to 3.2M and the initial OH/Zn ratio from 0.5 to 1.6 were used at temperatures from 20 to 60 °C. All samples were characterized in detail by X-ray diffraction, scanning electron microscopy, differential thermal analysis and ICP. Stability and distribution of the zinc hydroxide nitrate particles were estimated too.

Keywords: zinc hydroxide nitrate, nanoparticles, preparation, foliar fertilizer

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Authors: Jing-Yang Chung, Chi-Wei Liao, Jing Li, Bor Kae Chang, Cheng-Yu Wang

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Chemical hydride ammonia borane (AB, NH3BH3) draws attentions to hydrogen energy researches for its high theoretical gravimetrical capacity (19.6 wt%). Nevertheless, the elevated AB decomposition temperatures (Td) and unwanted byproducts are main hurdles in practical application. It was reported that the byproducts and Td can be reduced with nanoconfinement technique, in which AB molecules are confined in porous materials, such as porous carbon, zeolite, metal-organic frameworks (MOFs), etc. Although nanoconfinement empirically shows effectiveness on hydrogen generation temperature reduction in AB, the theoretical mechanism is debatable. Low Td was reported in AB@IRMOF-1 (Zn4O(BDC)3, BDC = benzenedicarboxylate), where Zn atoms form closed metal clusters secondary building unit (SBU) with no exposed active sites. Other than nanosized hydride, it was also observed that catalyst addition facilitates AB decomposition in the composite of Li-catalyzed carbon CMK-3, MOF JUC-32-Y with exposed Y3+, etc. It is believed that nanosized AB is critical for lowering Td, while active sites eliminate byproducts. Nonetheless, some researchers claimed that it is the catalytic sites that are the critical factor to reduce Td, instead of the hydride size. The group physically ground AB with ZIF-8 (zeolitic imidazolate frameworks, (Zn(2-methylimidazolate)2)), and found similar reduced Td phenomenon, even though AB molecules were not ‘confined’ or forming nanoparticles by physical hand grinding. It shows the catalytic reaction, not nanoconfinement, leads to AB dehydrogenation promotion. In this research, we explored the possible criteria of hydrogen production temperature from nanoconfined AB in MOFs with different pore sizes and active sites. MOFs with metal SBU such as Zn (IRMOF), Zr (UiO), and Al (MIL-53), accompanying with various organic ligands (BDC and BPDC; BPDC = biphenyldicarboxylate) were modified with AB. Excess MOFs were used for AB size constrained in micropores estimated by revisiting Horvath-Kawazoe model. AB dissolved in methanol was added to MOFs crystalline with MOF pore volume to AB ratio 4:1, and the slurry was dried under vacuum to collect AB@MOF powders. With TPD-MS (temperature programmed desorption with mass spectroscopy), we observed Td was reduced with smaller MOF pores. For example, it was reduced from 100°C to 64°C when MOF micropore ~1 nm, while ~90°C with pore size up to 5 nm. The behavior of Td as a function of AB crystalline radius obeys thermodynamics when the Gibbs free energy of AB decomposition is zero, and no obvious correlation with metal type was observed. In conclusion, we discovered Td of AB is proportional to the reciprocal of MOF pore size, possibly stronger than the effect of active sites.

Keywords: ammonia borane, chemical hydride, metal-organic framework, nanoconfinement

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Authors: Karolina Ordon, Sandrine Coste, Malgorzata Makowska-Janusik, Abdelhadi Kassiba

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Photocatalytic processes play key role in the production of a new source of energy (as hydrogen), design of self-cleaning surfaces or for the environment preservation. The most challenging task deals with the purification of water distinguished by high efficiency. In the mentioned process, organic pollutants in solutions are decomposed to the simple, non-toxic compounds as H2O and CO2. The most known photocatalytic materials are ZnO, CdS and TiO2 semiconductors with a particular involvement of TiO2 as an efficient photocatalysts even with a high band gap equal to 3.2 eV which exploit only UV radiation from solar emitted spectrum. However, promising material with visible light induced photoactivity was searched through the monoclinic polytype of BiVO4 which has energy gap about 2.4 eV. As required in heterogeneous photocatalysis, the high contact surface is required. Also, BiVO4 as photocatalyst can be optimized by increasing its surface area by achieving the mesoporous structure synthesize. The main goal of the present work consists in the synthesis and characterization of BiVO4 mesoporous thin film. The synthesis method based on sol-gel was carried out using a standard surfactants such as P123 and F127. The thin film was deposited by spin and dip coating method. Then, the structural analysis of the obtained material was performed thanks to X-ray diffraction (XRD) and Raman spectroscopy. The surface of resulting structure was investigated using a scanning electron microscopy (SEM). The computer simulations based on modeling the optical and electronic properties of bulk BiVO4 by using DFT (density functional theory) methodology were carried out. The semiempirical parameterized method PM6 was used to compute the physical properties of BiVO4 nanostructures. The Raman and IR absorption spectra were also measured for synthesized mesoporous material, and the results were compared with the theoretical predictions. The simulations of nanostructured BiVO4 have pointed out the occurrence of quantum confinement for nanosized clusters leading to widening of the band gap. This result overcame the relevance of nanosized objects to harvest wide part of the solar spectrum. Also, a balance was searched experimentally through the mesoporous nature of the films devoted to enhancing the contact surface as required for heterogeneous catalysis without to lower the nanocrystallite size under some critical sizes inducing an increased band gap. The present contribution will discuss the relevant features of the mesoporous films with respect to their photocatalytic responses.

Keywords: bismuth vanadate, photocatalysis, thin film, quantum-chemical calculations

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Authors: Lila A. Alkhattaby, Norah A. Alsayegh, Mohammad S. Ansari, Mohammad O. Ansari

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In this work, we doped zinc oxide ZnO with potassium K we have synthesized using the sol-gel method. Structural properties were depicted by X-ray diffractometer (XRD) and energy distribution spectroscopy, X-ray diffraction studies confirm the nanosized of the particles and favored orientations along the (100), (002), (101), (102), (110), (103), (200), and (112) planes confirm the hexagonal wurtzite structure of ZnO NPs. The optical properties study using the UV-Vis spectroscopy. The band gap decreases from 4.05 eV to 3.88 eV, the lowest band gap at 10% doped concentration. The photoluminescence (PL) spectroscopy results show two main peaks, a sharp peak at ≈ 384 nm in the UV region and a broad peak around 479 nm in the visible region. The highest intensity of the band-edge luminescence was for 2% doped concentration because of the combined effect of the decreased probability of nonradiative recombination and has better crystallinity.

Keywords: K doped ZnO, photoluminescence spectroscopy, UV-Vis spectroscopy, x-ray spectroscopy

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Authors: Ebtesam. E. Ateia, L. M. Salah, A. H. El-Bassuony

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The aim of the presented study was the possibility of developing a nanosized material with enhanced structural properties that was suitable for many applications. Nanostructure ferrite of composition Ni0.5 Zn0.5 Cr0.1 Fe1.9 O4 were prepared by sol–gel, co-precipitation, citrate-gel, flash and oxalate precursor methods. The Structural and micro structural analysis of the investigated samples were carried out. It was observed that the lattice parameter of cubic spinel was constant, and the positions of both tetrahedral and the octahedral bands had a fixed position. The values of the lattice parameter had a significant role in determining the stoichiometric cation distribution of the composition.The average crystalline sizes of the investigated samples were from 16.4 to 69 nm. Discussion was made on the basis of a comparison of average crystallite size of the investigated samples, indicating that the co-precipitation method was the the effective one in producing small crystallite sized samples.

Keywords: chemical preparation, ferrite, grain size, nanocomposites, sol-gel

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Authors: Iman Taraghi, Sandra Paszkiewicz, Daria Pawlikowska, Anna Szymczyk, Izabela Irska, Rafal Stanik, Amelia Linares, Tiberio A. Ezquerra, Elżbieta Piesowicz

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Currently, the massive use of thermoplastic materials in industrial applications causes huge amounts of polymer waste. The poly (ethylene glycol-co-1,4-cyclohexanedimethanol terephthalate) (PET-G) has been widely used in food packaging and polymer foils. In this research, the PET-G foils have been recycled and reused as a matrix to combine with different types of nanofillers such as carbon nanotubes, graphene nanoplatelets, and nanosized carbon black. The mechanical and electrical properties, as well as thermal stability and thermal conductivity of the PET-G, improved along with the addition of the aforementioned nanofillers and hybrid system of them.

Keywords: polymer hybrid nanocomposites, carbon nanofillers, recycling, physical performance

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Authors: A. Pourahmad, Sh. Gharipour

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The present work describes the preparation and characterization of nanosized SiO₂@PbS core-shell particles by using a simple wet chemical route. This method utilizes silica spheres formation followed by successive ionic layer adsorption and reaction method assisted lead sulphide shell layer formation. The final product was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis spectroscopic, infrared spectroscopy (IR) and transmission electron microscopy (TEM) experiments. The morphological studies revealed the uniformity in size distribution with core size of 250 nm and shell thickness of 18 nm. The electron microscopic images also indicate the irregular morphology of lead sulphide shell layer. The structural studies indicate the face-centered cubic system of PbS shell with no other trace for impurities in the crystal structure.

Keywords: core-shell, nanostructure, semiconductor, optical property, XRD

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Authors: M. Shopska, D. Paneva, G. Kadinov, Z. Cherkezova-Zheleva, I. Mitov

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The iron containing materials are used as catalysts in different processes. The chemical methods of their synthesis use toxic and expensive chemicals; sophisticated devices; energy consumption processes that raise their cost. Besides, dangerous waste products are formed. At present time such syntheses are out of date and wasteless technologies are indispensable. The bioinspired technologies are consistent with the ecological requirements. Different microorganisms participate in the biomineralization of the iron and some phytochemicals are involved, too. The methods for biogenic production of iron containing materials are clean, simple, nontoxic, realized at ambient temperature and pressure, cheaper. The biogenic iron materials embrace different iron compounds. Due to their origin these substances are nanosized, amorphous or poorly crystalline, porous and have number of useful properties like SPM, high magnetism, low toxicity, biocompatibility, absorption of microwaves, high surface area/volume ratio, active sites on the surface with unusual coordination that distinguish them from the bulk materials. The biogenic iron materials are applied in the heterogeneous catalysis in different roles - precursor, active component, support, immobilizer. The application of biogenic iron oxide materials gives rise to increased catalytic activity in comparison with those of abiotic origin. In our study we investigated the catalytic behavior of biomasses obtained by cultivation of Leptothrix bacteria in three nutrition media – Adler, Fedorov, and Lieske. The biomass composition was studied by Moessbauer spectroscopy and transmission IRS. Catalytic experiments on CO oxidation were carried out using in situ DRIFTS. Our results showed that: i) the used biomasses contain α-FeOOH, γ-FeOOH, γ-Fe2O3 in different ratios; ii) the biomass formed in Adler medium contains γ-FeOOH as main phase. The CO conversion was about 50% as evaluated by decreased integrated band intensity in the gas mixture spectra during the reaction. The main phase in the spent sample is γ-Fe2O3; iii) the biomass formed in Lieske medium contains α-FeOOH. The CO conversion was about 20%. The main phase in the spent sample is α-Fe2O3; iv) the biomass formed in Fedorov medium contains γ-Fe2O3 as main phase. CO conversion in the test reaction was about 19%. The results showed that the catalytic activity up to 200°C resulted predominantly from α-FeOOH and γ-FeOOH. The catalytic activity at temperatures higher than 200°C was due to the formation of γ-Fe2O3. The oxyhydroxides, which are the principal compounds in the biomass, have low catalytic activity in the used reaction; the maghemite has relatively good catalytic activity; the hematite has activity commensurate with that of the oxyhydroxides. Moreover it can be affirmed that catalytic activity is inherent in maghemite, which is obtained by transformation of the biogenic lepidocrocite, i.e. it has biogenic precursor.

Keywords: nanosized biogenic iron compounds, catalytic behavior in reaction of CO oxidation, in situ DRIFTS, Moessbauer spectroscopy

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Authors: A. V. Samokhin, A. A. Fadeev, M. A. Sinaiskii, N. V. Alekseev, A. V. Kolesnikov

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Composite materials where metal matrix is reinforced by ceramic or metal particles are of great interest for use in the manufacturing of electrical contacts. Significant improvement of the composite physical and mechanical properties as well as increase of the performance parameters of composite-based products can be achieved if the nanoscale structure in the composite materials is obtained by using nanosized powders as starting components. The results of nanosized composite powders synthesis (Ag-SnO2, W-Cu and Cu-C) in the DC thermal plasma flows are presented in this paper. The investigations included the following processes: - Recondensation of micron powder mixture Ag + SnO2 in a nitrogen plasma; - The reduction of the oxide powders mixture (WO3 + CuO) in a hydrogen-nitrogen plasma; - Decomposition of the copper formate and copper acetate powders in nitrogen plasma. The calculations of equilibrium compositions of multicomponent systems Ag-Sn-O-N, W-Cu-O-H-N and Cu-O-C-H-N in the temperature range of 400-5000 K were carried to estimate basic process characteristics. Experimental studies of the processes were performed using a plasma reactor with a confined jet flow. The plasma jet net power was in the range of 2 - 13 kW, and the feedstock flow rate was up to 0.35 kg/h. The obtained powders were characterized by TEM, HR-TEM, SEM, EDS, ED-XRF, XRD, BET and QEA methods. Nanocomposite Ag-SnO2 (12 wt. %). Processing of the initial powder mixture (Ag-SnO2) in nitrogen thermal plasma stream allowed to produce nanopowders with a specific surface area up to 24 m2/g, consisting predominantly of particles with size less than 100 nm. According to XRD results, tin was present in the obtained products as SnO2 phase, and also as intermetallic phases AgxSn. Nanocomposite W-Cu (20 wt .%). Reduction of (WO3+CuO) mixture in the hydrogen-nitrogen plasma provides W-Cu nanopowder with particle sizes in the range of 10-150 nm. The particles have mainly spherical shape and structure tungsten core - copper shell. The thickness of the shell is about several nanometers, the shell is composed of copper and its oxides (Cu2O, CuO). The nanopowders had 1.5 wt. % oxygen impurity. Heat treatment in a hydrogen atmosphere allows to reduce the oxygen content to less than 0.1 wt. %. Nanocomposite Cu-C. Copper nanopowders were found as products of the starting copper compounds decomposition. The nanopowders primarily had a spherical shape with a particle size of less than 100 nm. The main phase was copper, with small amount of Cu2O and CuO oxides. Copper formate decomposition products had a specific surface area 2.5-7 m2/g and contained 0.15 - 4 wt. % carbon; and copper acetate decomposition products had the specific surface area 5-35 m2/g, and carbon content of 0.3 - 5 wt. %. Compacting of nanocomposites (sintering in hydrogen for Ag-SnO2 and electric spark sintering (SPS) for W-Cu) showed that the samples having a relative density of 97-98 % can be obtained with a submicron structure. The studies indicate the possibility of using high-intensity plasma processes to create new technologies to produce nanocomposite materials for electric contacts.

Keywords: electrical contact, material, nanocomposite, plasma, synthesis

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Authors: N. Hasbullah, K. A. Sekak

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The sulfonated poly (ether ether ketone) SPEEK nanofiber membrane were successfully electrospun for Polymer Electrolyte Membrane (PEM) in Proton Exchange Membrane Fuel Cell (PEMFC) and their nanosized properties were investigated. The poly (ether ether ketone) PEEK victrex® grade 90p was sulfonated with concentrated sulfuric acid (95-98% w/w) at room temperature for 60 hours sulfonation times. The degree sulfonation of SPEEK are 70% was determined by H1 NMR and the functional groups of the SPEEK were characterize using FTIR. Then, the SPEEK nanofiber membrane were prepared via electrospinning method using DMAC as a solvent. The SPEEK sample were successfully electrospun using predetermine set up. FESEM show the electrospun fiber mat surface and confirmed the nanostructure membrane cell.

Keywords: polymer electrolyte membrane (PEM), sulfonated poly (ether ether ketone) (SPEEK), degree sulfonation, Electrospinning, Nanofibers

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Authors: Preeti Makkar, R. C. Agarwala, Vijaya Agarwala

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The present study focuses on the preparation of Al2O3 nanoparticles by top down approach i.e. mechanical milling using high energy planetary ball mill at 250 rpm for 40h. The milled Al2O3 nanoparticles are then used as the second phase to develop electroless (EL) Ni-P- Al2O3 nanocomposite coatings on mild steel substrate. An alkaline bath was used with a suspension of Al2O3 particles (4 g/L) for the synthesis of Ni-P-Al2O3 nanocomposite coating. The surface morphology, size range and phase analysis of as-prepared Al2O3 particles and the coatings were characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The coatings were heat treated at 400°C for 1h in argon atmosphere and the hardness of the nanocomposite coatings was investigated with respect to Ni-P before and after heat treatment. The results showed that as milled Al2O3 nanoparticles exhibit irregular shaped and size ranges around 40-45 nm. The Al2O3 particles are uniformly distributed in Ni-P matrix. The microhardness of the coatings is found to be significantly improved after heat treatment (1126 VHN).

Keywords: Electroless (EL), Ni-P-Al2O3, nanocomposite, mechanical milling, microhardness

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Authors: Radhiyatul Hikmah Binti Abu, Zukhairi Bin Md Rahim, Siti Ujila Binti Masuri, Nur Ismarrubie Binti Zahari, Mohd Zobir Hussein

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This paper describes the synthesis of Calcium Diethylenetriamine-penta (Ca-DTPMP) Scale Inhibitor (SI) and the effect of temperature on its adsorption onto the mineral surfaces. Nanosized particles of Ca-DTPMP SI were synthesized and TEM result shows that the sizes of the synthesized particles are ranged from 10 nm to 30 nm. This synthesized nano SI was then used in static adsorption/precipitation test with various temperatures (37°C, 60°C and 100°C) to determine the effect of temperature on its adsorption ability. The performance of the SI was measured by their diffusion capability, which can be inferred by weighing the metal-SI that successfully adsorbed onto the kaolinite (mineral) surface. The kaolinite samples were analyzed using Scanning Electron Microscope (SEM) and the results show the reduction of pores on kaolinite surface as temperature increases. This indicates higher adsorption of the SI particles onto the mineral surface. Furthermore, EDX analysis shows the presence of Phosphorus (P) and Magnesium (Mg2+) on kaolinite particle surface, hence reaffirming the fact that adsorption took place on the kaolinite surface.

Keywords: adsorption, diffusivity, scale, scale inhibitor

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Authors: Nguyen Cao Nguyen, Krasimir I. Ivanov, Penka S. Zapryanova

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The present study was carried out to investigate the interaction of foliar applied zinc with other elements in Phyllanthus amarus plants. The plant samples for our experiment were collected from Lam Dong province, Vietnam. Seven suspension solutions of nanosized zinc hydroxide nitrate (Zn₅(OH)₈(NO₃)₂·2H₂O) with different Zn concentration were used. Fertilization and irrigation were the same for all variants. The Zn content and the content of selected micro (Cu, Fe, Mn) and macro (Ca, Mg, P and K) nutrients in plant roots, and stems and leaves were determined. It was concluded that the zinc content of plant roots varies narrowly, with no significant impact of ZnHN fertilization. The same trend can be seen in the content of Cu, Mn, and macronutrients. The zinc content of plant stems and leaves varies within wide limits, with the significant impact of ZnHN fertilization. The trends in the content of Cu, Mn, and macronutrients are kept the same as in the root, whereas the iron trends to increase its content at increasing the zinc content.

Keywords: Phyllanthus amarus, Zinc, Micro and macro elements, foliar fertilizer

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Authors: Sucharat Limsitthichaikoon, Kedsarin Saodaeng, Aroonsri Priprem, Teerasak Damrongrungruang

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Complexation of anthocyanins to mimic natural copigmentation process was investigated. Cyanidin-rich extracts from Zea mays L. CeritinaKulesh. anddelphinidin-rich extracts from ClitoriaternateaL. were used to form 4 anthocyanin complexes, AC1, AC2, AC3, and AC4, in the presence of several polyphenols and a trace metal. Characterizations of the ACs were conducted by UV, FTIR, DSC/TGA and morphological observations. Bathochromic shifts of the UV spectra of 4 formulas of ACs were observed at peak wavelengths of about 510-620 nm by 10 nm suggesting complex formation.FTIR spectra of the ACs indicate shifts of peaks from 1,733 cm-1 to 1,696 cm-1 indicating interactions and a decrease in the peak areas within the wavenumber of 3,400-3,500 cm-1 indicating changes in hydrogen bonding.Thermal analysis of all of the ACs suggests increases in melting temperature after complexation. AC with the highest melting temperature was morphologically observed by SEM and TEM to be crystal-like particles within a range of 50 to 200 nm. Particle size analysis of the AC by laser diffraction gave a range of 50-600 nm, indicating aggregation. This AC was shown to have no cytotoxic effect on cultured HGEPp0.5 and HGF (all p> 0.05) by MTT. Therefore, complexation of anthocyanins was simple and self-assembly process, potentially resulting in nanosized particles of anthocyanin complex.

Keywords: anthocyanins, complexation, purple corn cops, butterfly pea, physicochemical characteristics, cytotoxicity

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Authors: Sergei Zhevnenko

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Сontinuous layer of tantalum boride is formed on the surface as a result of reactive wetting of oxidized tantalum by copper melt with boron at a temperatures above 1150 °C. An increase in the wetting temperature above 1400 °C leads to a change in the formation mechanism of tantalum borides, they are formed in the nanosized flakes. In the presented work, we studied the process of copper-based in-situ composite formation, strengthened by the particles of tantalum borides. We investigated the structure of the formed particles, the conditions, and the kinetics of their formation. Dissolving boride particles do not have time to mix uniformly in the melt upon sufficiently rapid cooling and form a macrostructure, partly repeating the shape of the metallic tantalum. This allows to set different gradient structures in the copper alloy. Such macrostructures have been obtained. Boride particles and microstructures were studied by scanning and transmission electron microscopy, and regions with particles were investigated by nanoindentation. In this work, we also measured the kinetics of impregnation of porous tantalum with copper-boron melt and studied the structures of the composite, in which the melt filling the interpore space is saturated with boride particles.

Keywords: copper, tantalum borides, in-situ composites, wetting, imbibition

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Authors: Shalini Rajput, Dinesh Mohan

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Water is the most important and essential resources for existing of life on the earth. Water quality is gradually decreasing due to increasing urbanization and industrialization and various other developmental activities. It can pose a threat to the environment and public health therefore it is necessary to remove hazardous contaminants from wastewater prior to its discharge to the environment. Recently, magnetic iron oxide nanoparticles have been arise as significant materials due to its distinct properties. This article focuses on the synthesis method with a possible mechanism, structure and application of magnetic iron oxide nanoparticles. The various characterization techniques including X-ray diffraction, transmission electron microscopy, scanning electron microscopy with energy dispersive X-ray, Fourier transform infrared spectroscopy and vibrating sample magnetometer are useful to describe the physico-chemical properties of nanoparticles. Nanosized iron oxide particles utilized for remediation of contaminants from aqueous medium through adsorption process. Due to magnetic properties, nanoparticles can be easily separate from aqueous media. Considering the importance and emerging trend of nanotechnology, iron oxide nanoparticles as nano-adsorbent can be of great importance in the field of wastewater treatment.

Keywords: nanoparticles, adsorption, iron oxide, nanotechnology

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Authors: Sabrina Boutaleb, Fouad Bourad, Kouider Halim Benrahou, Abdelouahed Tounsi

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In the present work, the dynamic analysis of the functionally graded rectangular nanoplates is studied. The theory of nonlocal elasticity based on the quasi 3D high shear deformation theory (quasi 3D HSDT) has been employed to determine the natural frequencies of the nanosized FG plate. In HSDT, a cubic function is employed in terms of thickness coordinates to introduce the influence of transverse shear deformation and stretching thickness. The theory of nonlocal elasticity is utilized to examine the impact of the small scale on the natural frequency of the FG rectangular nanoplate. The equations of motion are deduced by implementing Hamilton’s principle. To demonstrate the accuracy of the proposed method, the calculated results in specific cases are compared and examined with available results in the literature, and a good agreement is observed. Finally, the influence of the various parameters, such as the nonlocal coefficient, the material indexes, the aspect ratio, and the thickness-to-length ratio, on the dynamic properties of the FG nanoplates is illustrated and discussed in detail.

Keywords: nonlocal elasticity theory, FG nanoplate, free vibration, refined theory, elastic foundation

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Authors: Jenaidullah Batur, Sebghatullah Mudaber

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Currently, there is a list of catalysts that can reduce CO₂ to valuable chemicals and fuels, among them metal oxides such as TiO₂, known as promising photocatalysts to produce hydrogen and CO unless they are at an earlier age and still need to promote activity to able for produce fabricated values. Herein, in this work, we provided a novel, facile and eco-friendly synthesis strategy to synthesize more effective TiO₂-organic composite materials to selectively reduce CO₂ to CO. In this experiment, commercial nanocrystalline TiO₂ and saccharin with Li (LiBr, LiCl) were synthesized using the facile physical grinding in the motel pestle for 10 minutes, then added 10 mL of deionized water (18.2 megaohms) on the 300mg composite catalyst before samples moving for hydrothermal heating for 24 hours at 80 C in the oven. Compared with nanosized TiO₂, the new TiO₂-Sac-Li indeed displays a high CO generation rate of 70.83 μmol/g/h, which is 7 times higher than TiO₂, which shows enhancement in CO₂ reduction and an apparent improvement in charge carrier dynamic. The CO₂ reduction process at the gas-solid interface on TiO₂-Sac-Li composite semiconductors is investigated by functional calculations and several characterization methods. The results indicate that CO₂ can be easily activated by the TiO₂-Sac-Li atoms on the surface. This work innovatively investigates CO₂ reduction in novel composite materials and helps to broaden the applications of composite materials semiconductors.

Keywords: green chemistry, green synthesis, TiO₂, photocatalyst

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Authors: H. Merzouka, D. T. Talantikitea, S. Fettouchib, L. Nessarkb

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Recently New nanosized materials studies are in huge expansion worldwide. They play a fundamental role in various industrial applications thanks their unique and functional properties. Moreover, in recent years, a great effort has been made in design and control fabrication of nano-structured semiconductors such as zinc sulphide. In recent years, much attention has been accorded in doped and co-doped ZnS to improve the ZnS films quality. We present in this work preparation and characterization of ZnS and Cu doped ZnS thin films. Nanoparticles ZnS and Cu doped ZnS films are prepared by chemical bath deposition method (CBD), for various dopant concentrations. Thin films are deposed onto commercial microscope glass slides substrates. Thiourea is used as sulfide ion source, zinc acetate as zinc ion source and copper acetate as Cu ion source in alkaline bath at 90 °C. X-ray diffraction (XRD) analyses are carried out at room temperature on films and powders with a powder diffractometer, using CuK radiation. The average grain size obtained from the Debye–Scherrer’s formula is around 10 nm. Films morphology is examined by scanning electron microscopy. IR spectra of representative sample are recorded with the FTIR between 400 and 4000 cm-1. The transmittance is more than 70 % is performed with the UV–VIS spectrometer in the wavelength range 200–800 nm. This value is enhanced by Cu doping.

Keywords: Cu doped ZnS, nanostructured, thin films, CBD, XRD, FTIR

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Authors: Hamid Merzouk, Djahida Touati-Talantikite, Amina Zaabar

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New nanosized materials are in huge expansion worldwide. They play a fundamental role in various industrial applications thanks their unique and functional properties. Moreover, in recent years, a great effort has been made to the design and control fabrication of nanostructured semiconductors such zinc sulphide. In recent years, much attention has been accorded in doped and co-doped ZnS to improve the ZnS films quality. We present in this work the preparation and characterization of ZnS and Al doped ZnS thin films. Nanoparticles ZnS and Al doped ZnS films are prepared by chemical bath deposition method (CBD), for various dopant concentrations. Thin films are deposed onto commercial microscope glass slides substrates. Thiourea is used as sulfide ion source, zinc acetate as zinc ion source and manganese acetate as manganese ion source in alkaline bath at 90 °C. X-ray diffraction (XRD) analyses are carried out at room temperature on films and powders with a powder diffractometer, using CuKα radiation. The average grain size obtained from the Debye–Scherrer’s formula is around 10 nm. Films morphology is examined by scanning electron microscopy. IR spectra of representative sample are recorded with the FTIR between 400 and 4000 cm-1.The transmittance (70 %) is performed with the UV–VIS spectrometer in the wavelength range 200–800 nm. This value is enhanced by Al doping.

Keywords: ZnS, nanostructured semiconductors, thin films, chemical bath deposition

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Authors: Kun Liang Ang, Eng Toon Saw, Wei He, Xuecheng Dong, Seeram Ramakrishna

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Ester solvents are widely used in pharmaceutical, printing and flavor industry due to their good miscibility, low toxicity, and high volatility. Through pervaporation, these ester solvents can be recovered from industrial wastewater. While metal-doped silicalite 1 zeolite membranes are commonly used in organic solvent recovery in the pervaporation process, these ceramic membranes suffer from low membrane permeation flux, mainly due to the high thickness of the metal-doped zeolite membrane. Herein, a simple method of fabricating an ultrathin tin-silicalite 1 membrane supported on alumina tube is reported. This ultrathin membrane is able to achieve high permeation flux and separation factor for an ester in a diluted aqueous solution. Nanosized tin-Silicalite 1 seeds which are smaller than 500nm has been formed through hydrothermal synthesis. The sn-Silicalite 1 seeds were then seeded onto alumina tube through dip coating, and the tin-Silicalite 1 membrane was then formed by hydrothermal synthesis in an autoclave through secondary growth method. Multiple membrane synthesis factors such as seed size, ceramic substrate surface pore size selection, and secondary growth conditions were studied for their effects on zeolite membrane growth. The microstructure, morphology and the membrane thickness of tin-Silicalite 1 zeolite membrane were examined. The membrane separation performance and stability will also be reported.

Keywords: ceramic membrane, pervaporation, solvent recovery, Sn-MFI zeolite

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Authors: Kirandeep Kaur, Rohit Mehra, Pargin Bangotra

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Radon and thoron are pervasive radioactive gases and so are their progenies. The progenies of radon and thoron are present in the indoor atmosphere as attached/unattached fractions. In the present work, seasonal variation of concentration of attached and total (attached + unattached) nanosized decay products of indoor radon and thoron has been studied in the dwellings of Bathinda District of Punjab using Deposition based progeny sensors over long integrated times, which are independent of air turbulence. The preliminary results of these measurements are reported particularly regarding DTPS (Direct Thoron Progeny Sensor) and DRPS (Direct Radon Progeny Sensor) for the first time in Bathinda. It has been observed that there is a strong linear relationship in total EERC (Equilibrium Equivalent Radon Concentration) and EETC (Equilibrium Equivalent Thoron Concentration) in rainy season (R2 = 0.83). Further a strong linear relation between total indoor radon concentration and attached fraction has also been observed for the same rainy season (R2= 0.91). The concentration of attached progeny of radon (EERCatt) is 76.3 % of the total Equilibrium Equivalent Radon Concentration (EERC).

Keywords: radon, thoron, progeny, DTPS/DRPS, EERC, EETC, seasonal variation

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Authors: Hanjie Xie, Raphael Semiat, Ziyi Zhong

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It is well known that many oxidation reactions in nature are closely related to the origin and life activities. One of the features of these natural reactions is that they can proceed under mild conditions employing the oxidant of molecular oxygen (O₂) in the air and enzymes as catalysts. Catalysis is also a necessary part of life for human beings, as many chemical and pharmaceutical industrial processes need to use catalysts. However, most heterogeneous catalytic reactions must be run at high operational reaction temperatures and pressures. It is not strange that, in recent years, research interest has been redirected to green catalysis, e.g., trying to run catalytic reactions under relatively mild conditions as much as possible, which needs to employ green solvents, green oxidants such O₂, particularly air, and novel catalysts. This work reports the efficient binary Fe-Mn metal oxide catalysts for low-temperature formaldehyde (HCHO) oxidation, a toxic pollutant in the air, particularly in indoor environments. We prepared a series of nanosized FeMn oxide catalysts and found that when the molar ratio of Fe/Mn = 1:1, the catalyst exhibited the highest catalytic activity. At room temperature, we realized the complete oxidation of HCHO on this catalyst for 20 h with a high GHSV of 150 L g⁻¹ h⁻¹. After a systematic investigation of the catalyst structure and the reaction, we identified the reaction intermediates, including dioxymethylene, formate, carbonate, etc. It is found that the oxygen vacancies and the derived active oxygen species contributed to this high-low-temperature catalytic activity. These findings deepen the understanding of the catalysis of these binary Fe-Mn metal oxide catalysts.

Keywords: oxygen vacancy, catalytic oxidation, binary transition oxide, formaldehyde

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Authors: Masoumeh Tabatabaee, Zahra Shahryarzadeh, Masoud R. Shishebor

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Advanced oxidation process (AOPs) is alternative method for the complete degradation many organic pollutants. When a photocatalyst absorbs radiation whose energy hν > Eg an ē from its filled valance band (VB) is promoted to its conduction band (CB) and valance band holes h+ are formed. Electron would reduce any available species, including O2, water and hydroxide ion to form hydroxyl radicals. ZnO and TiO2 are important photocatalysts with high catalytic activity that have attracted much research attention. TiO2 can only absorb a small portion of solar spectrum in the UV region and many methods such as dye sensitization, doping of other metals and using TiO2 with another semiconductor have been used to improve the photocatalytic activity of TiO2 under solar irradiation. Studies have shown that the use of metal oxides or sulfide such as WO3, MoO3, SiO2, MgO, ZnO, and CdS with TiO2 can significantly enhance the photocatalytic activity of TiO2. Due to similarity of photodegradation mechanism of ZnO with TiO2, it is a suitable semiconductor using with TiO2 and recently nanosized bicomponent TiO2-ZnO photocatalysts were prepared and used for degradation of some pollutants. In this study, Nano-sized ZnO/TiO2 composite was synthesized. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the structure and morphology of it. The effect of photocatalytic activity of prepared ZnO/TiO2 on the degradation of cyanide ion under UV was investigated. The effect of various parameters such as ZnO/TiO2 concentration, amount of photocatalyst, amount of H2O2, initial dye or cyanide ion concentration, pH and irradiation time on were investigated. Results show that more than 95% of 4 mgL-1 cyanide ion degraded after 60-min reaction time and under UV irradiation.

Keywords: photodegradation, ZnO/TiO2, nanoparticle, cyanide ion

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Authors: I. Yordanova, H. Kolev, S. Todorova, Z. Cherkezova-Zheleva

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Catalysis plays a key role in solving many environmental problems by establishing efficient catalytic systems for environmental protection and reducing emissions of greenhouse gases from industry. Volatile organic compounds are major air pollutants. There are several ways to dispose of emissions like - adsorption, condensation, absorption, bio-filtration, thermal, catalytic, plasma and ultraviolet oxidation. The catalytic oxidation has more advantages over other methods. For example - lower energy consumption; the concentration of the organic contaminant may be low or may vary within wide limits. Catalysts for complete oxidation of VOCs can be classified into three categories: noble metal, metal oxides or supported metal oxides and mixture of noble metals and metal oxides. Most of the catalysts for the complete catalytic oxidation are based on Pt, Pd, Rh or a combination thereof. The oxides of the transition metal are one of the alternatives to noble metal catalysts for these reactions. They are less active at low temperatures, but at higher - their activity is similar. The properties of the catalyst depend on the distribution of the active phase, the medium type of the pre-treatment, the interaction between the active phase and the support and the interaction between the active phase and the reaction medium. Supported mono-component Mn and bi-component Mn-Co systems are examined in present study. The samples are prepared using co-precipitation method. SiO2 (Aerosil) is used as a support. The studied samples were precipitated by NH4OH. The synthesized samples were characterized by XRD, XPS, TPR and tested in the catalytic reaction of complete oxidation of n-hexane, propane, methanol, ethanol and propanol.

Keywords: catalytic oxidation, Co-Mn oxide, oxidation of hydrocarbons and alcohols, environmental protection

Procedia PDF Downloads 362