Preparation of Nanocrystalline Mesoporous ThO2 via Surfactant Assisted Sol-gel Procedure

In this research, thorium dioxide mesoporous nanocrystalline powder was synthesized through the sol-gel method using hydrated thorium nitrate and ammonium hydroxide as starting materials and Triton X100 as surfactant. ThO2 gel was characterized by thermogravimetric (TGA), and prepared ThO2 powder was subjected to scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer-Emett-Teller (BET) analyses studies. Detailed analyses show that prepared powder consisted of phase with the space group Fm3m of thoria and its crystalline size was 12.6 nm. The thoria possesses 16.7 m2/g surface area and the pore volume and size calculated to be 0.0423 cc/g and 1.947 nm, respectively.

The Mechanical and Electrochemical Properties of DC-Electrodeposited Ni-Mn Alloy Coating with Low Internal Stress

The nickel-manganese (Ni-Mn) alloy coating prepared from DC electrodeposition process in sulphamate bath was studied. The effects of process parameters, such as current density and electrolyte composition, on the cathodic current efficiency, microstructure, internal stress and mechanical properties were investigated. Because of its crucial effect on the application to the electroforming of microelectronic components, the development of low internal stress coating with high leveling power was emphasized. It was found that both the coating’s manganese content and the cathodic current efficiency increased with the raise in current density. In addition, the internal stress of the deposited coating showed compressive nature at low current densities while changed to tensile one at higher current densities. Moreover, the metallographic observation, X-ray diffraction measurement, and polarization curve measurement were conducted. It was found that the Ni-Mn coating consisted of nano-sized columnar grains and the maximum hardness of the coating was associated with (111) preferred orientation in the microstructure. The grain size was refined along with the increase in the manganese content of the coating, which accordingly, raised its hardness and resistance to annealing softening. In summary, the Ni-Mn coating prepared at lower current density of 1-2 A/dm2 had low internal stress, high leveling power, and better corrosion resistance.

Preparation of Protective Coating Film on Metal Alloy

A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in – situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physicochemical properties were investigated using X-ray diffraction (XRD), Electron Microscopy (SEM), Energy Dispersive X–ray Analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC).

Synthesizing CuFe2O4 Spinel Powders by a Combustion-Like Process for Solid Oxide Fuel Cell Interconnect Coatings

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

Preparation and Characterization of Polyaniline (PANI)-Platinum Nanocomposite

Polyaniline is an indispensible component in lightemitting devices (LEDs), televisions, cellular telephones, automotive, corrosion-resistant coatings, actuators etc. The electrical conductivity properties was found be increased by introduction of metal nano particles. In the present study, an attempt has been made to utilize platinum nano particles to achieve the improved electrical properties. Polyaniline and Pt-polyaniline composite are synthesized by electrochemical routes. X-ray diffractometer confirms the amorphous nature of polyaniline. The Bragg’s diffraction peaks correspond to platinum nanoparticles in Pt-polyaniline composite and thermogravimetric analyzer indicates its decomposition at certain temperature. The Scanning Electron Micrographs of colloidal platinum nanoparticles were spherical, uniform shape in the composite. The current-voltage (I-V) characteristics of the PANI and composites were also studied which indicate a significant decreasing resistivity than PANI-Platinum after introduction of pt nanoparticles in the matrix of polyaniline (PANI).

Thermo-Mechanical Treatments of Cu-Ti Alloys

This paper aims to study the effect of cold work condition on the microstructure of Cu-1.5wt%Ti, and Cu-3.5wt%Ti and hence mechanical properties. The samples under investigation were machined, and solution heat treated. X-ray diffraction technique is used to identify the different phases present after cold deformation by compression and also different heat treatment and also measuring the relative quantities of phases present. The metallographic examination is used to study the microstructure of the samples. The hardness measurements were used to indicate the change in mechanical properties. The results are compared with the mechanical properties obtained by previous workers. Experiments on cold compression followed by aging of Cu-Ti alloys have indicated that the most efficient hardening of the material results from continuous precipitation of very fine particles within the matrix. These particles were reported to be β`-type, Cu4Ti phase. The β`-β transformation and particles coarsening within the matrix as well as long grain boundaries were responsible for the overaging of Cu-1.5wt%Ti and Cu-3.5wt%Ti alloys. It is well known that plate-like particles are β – type, Cu3Ti phase. Discontinuous precipitation was found to start at the grain boundaries and expand into grain interior. At the higher aging temperature, a classic Widmanstätten morphology forms giving rise to a coarse microstructure comprised of α and the equilibrium phase β. Those results were confirmed by X-ray analysis, which found that a few percent of Cu3Ti, β precipitates are formed during aging at high temperature for long time for both Cu- Ti alloys (i.e. Cu-1.5wt%Ti and Cu-3.5wt%Ti).

Crystalline Structure of Starch Based Nano Composites

In contrast with literal meaning of nano, researchers have been achieved mega adventures in this area and every day more nanomaterials are being introduced to the market. After long time application of fossil-based plastics, nowadays accumulation of their waste seems to be a big problem to the environment. On the other hand, mankind has more attention to safety and living environment. Replacing common plastic packaging materials with degradable ones that degrade faster and convert to non-dangerous components like water and carbon dioxide have more attractions; these new materials are based on renewable and inexpensive sources of starch and cellulose. However, the functional properties of them do not suitable for packaging. At this point, nanotechnology has an important role. Utilizing of nanomaterials in polymer structure will improve mechanical and physical properties of them; nanocrystalline cellulose (NCC) has this ability. This work has employed a chemical method to produce NCC and starch bio nanocomposite containing NCC. X-Ray Diffraction technique has characterized the obtained materials. Results showed that applied method is a suitable one as well as applicable one to NCC production.

The Determination of the Potassium Nitrate, Sodium Hydroxide and Boric Acid Molar Ratio in the Synthesis of Potassium Borates via Hydrothermal Method

Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Raman Spectroscopy. The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8·4H2O) was synthesized as best.

Chitosan Functionalized Fe3O4@Au Core-Shell Nanomaterials for Targeted Drug Delivery

Chitosan functionalized Fe3O4-Au core shell nanoparticles have been prepared using a two-step wet chemical approach using NaBH4 as reducing agent for formation of Au in ethylene glycol. X-ray diffraction studies shows individual phases of Fe3O4 and Au in the as prepared samples with crystallite size of 5.9 and 11.4 nm respectively. The functionalization of the core-shell nanostructure with Chitosan has been confirmed using Fourier transform infrared spectroscopy along with signatures of octahedral and tetrahedral sites of Fe3O4 below 600cm-1. Mössbauer spectroscopy shows decrease in particle-particle interaction in presence of Au shell (72% sextet) than pure oleic coated Fe3O4 nanoparticles (88% sextet) at room temperature. At 80K, oleic acid coated Fe3O4 shows only sextets whereas the Chitosan functionalized Fe3O4 and Chitosan functionalized Fe3O4@Au core shell show presence of 5 and 11% doublet, respectively.

Influence of MgO Physically Mixed with Tungsten Oxide Supported Silica Catalyst on Coke Formation

The effect of additional magnesium oxide (MgO) was investigated by using the tungsten oxide supported on silica catalyst (WOx/SiO2) physically mixed with MgO in a weight ratio 1:1. The both fresh and spent catalysts were characterized by FT-Raman spectrometer, UV-Vis spectrometer, X-Ray diffraction (XRD) and temperature programmed oxidation (TPO). The results indicated that the additional MgO could enhance the conversion of trans-2-butene due to isomerization reaction. However, adding MgO would increase the amount of coke deposit on the WOx/SiO2 catalyst. The TPO profile presented two peaks when the WOx/SiO2 catalyst was physically mixed with MgO. The further peak was suggested that came from coke precursor could be produced by isomerization reaction of undesired product. Then, the occurred coke precursor could deposit and form coke on the acid catalyst.

Microstructural and Magnetic Properties of Ni50Mn39Sn11 and Ni50Mn36Sn14 Heusler Alloys

We report the microstructural and magnetic properties of Ni50Mn39Sn11 and Ni50Mn36Sn14 ribbon Heusler alloys. Experimental results were obtained by differential scanning calorymetry, X-ray diffraction and vibrating sample magnetometry techniques. The Ni-Mn-Sn system undergoes a martensitic structural transformation in a wide temperature range. For example, for Ni50Mn39Sn11 the start and finish temperatures of the martensitic and austenite phase transformation for ribbon alloy were Ms=336K, Mf=328K, As=335K and Af=343K whereas no structural transformation is observed for Ni50Mn36Sn14 alloys. Magnetic measurements show the typical ferromagnetic behavior with Curie temperature 207 K at low applied field of 50 Oe. The complex behavior exhibited by these Heusler alloys should be ascribed to the strong coupling between magnetism and structure, being their magnetic behavior determined by the distance between Mn atoms.

The Preparation of Silicon and Aluminum Extracts from Tuncbilek and Orhaneli Fly Ashes by Alkali Fusion

Coal fly ash is formed as a solid waste product from the combustion of coal in coal fired power stations. Huge amounts of fly ash are produced globally every year and are predicted to increase. Nowadays, less than half of the fly ash is used as a raw material for cement manufacturing, construction and the rest of it is disposed as a waste causing yet another environmental concern. For this reason, the recycling of this kind of slurries into useful materials is quite important in terms of economical and environmental aspects. The purpose of this study is to evaluate the Orhaneli and Tuncbilek coal fly ashes for utilization in some industrial applications. Therefore the mineralogical and chemical compositions of these fly ashes were analyzed by X-ray fluorescence spectroscopy, ourier-transform infrared spectrometer, and X-ray diffraction. The silicon (Si) and aluminum (Al) in the fly ashes were activated by alkali fusion technique with sodium hydroxide. The obtained extracts were analyzed for Si and Al content by inductively coupled plasma optical emission spectrometry.

Production of Composite Materials by Mixing Chromium-Rich Ash and Soda-Lime Glass Powder: Mechanical Properties and Microstructure

A chromium-loaded ash originating from incineration of tannery sludge under anoxic conditions was mixed with low grade soda-lime glass powder coming from commercial glass bottles. The relative weight proportions of ash over glass powder tested were 30/70, 40/60 and 50/50. The solid mixtures, formed in green state compacts, were sintered at the temperature range of 800o C up to 1200o C. The resulting products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDXS) and micro-indentation. The above methods were employed to characterize the various phases, microstructure and hardness of the produced materials. Thermal treatment at 800o C and 1000o C produced opaque ceramic products composed of a variety of chromium-containing and chromium-free crystalline phases. Thermal treatment at 1200o C gave rise to composite products, where only chromium-containing crystalline phases were detected. Hardness results suggest that specific products are serious candidates for structural applications.

Strengthening and Toughening of Dental Porcelain by the Inclusion of an Yttria-Stabilized Zirconia Reinforcing Phase

Dental porcelain composites reinforced and toughened by 20 wt.% tetragonal zirconia (3Y-TZP) were processed by hot pressing at 1000°C. Two types of particles were tested: yttriastabilized zirconia (ZrO2–3%Y2O3) agglomerates and pre-sintered yttria-stabilized zirconia (ZrO2–3%Y2O3) particles. The composites as well as the reinforcing particles were analyzed by the means of optical and Scanning Electron Microscopy (SEM), Energy Dispersion Spectroscopy (EDS) and X-Ray Diffraction (XRD). The mechanical properties were obtained by the transverse rupture strength test. Wear tests were also performed on the composites and monolithic porcelain. The best mechanical results were displayed by the porcelain reinforced with the pre-sintered ZrO2–3%Y2O3 agglomerates.

Carbamazepine Co-crystal Screening with Dicarboxylic Acids Co-Crystal Formers

Co-crystal is believed to improve the solubility and dissolution rates and thus, enhanced the bioavailability of poor water soluble drugs particularly during the oral route of administration. With the existing of poorly soluble drugs in pharmaceutical industry, the screening of co-crystal formation using carbamazepine (CBZ) as a model drug compound with dicarboxylic acids co-crystal formers (CCF) namely fumaric (FA) and succinic (SA) acids in ethanol has been studied. The co-crystal formations were studied by varying the mol ratio values of CCF to CBZ to access the effect of CCF concentration on the formation of the co-crystal. Solvent evaporation, slurry and cooling crystallization which representing the solution based method co-crystal screening were used. Based on the differential scanning calorimetry (DSC) analysis, the melting point of CBZ-SA in different ratio was in the range between 188oC-189oC. For CBZ-FA form A and CBZ-FA form B the melting point in different ratio were in the range of 174oC-175oC and 185oC-186oC respectively. The product crystal from the screening was also characterized using X-ray powder diffraction (XRPD). The XRPD pattern profile analysis has shown that the CBZ co-crystals with FA and SA were successfully formed for all ratios studied. The findings revealed that CBZ-FA co-crystal were formed in two different polymorphs. It was found that CBZ-FA form A and form B were formed from evaporation and slurry crystallization methods respectively. On the other hand, in cooling crystallization method, CBZ-FA form A was formed at lower mol ratio of CCF to CBZ and vice versa. This study disclosed that different methods and mol ratios during the co-crystal screening can affect the outcome of co-crystal produced such as polymorphic forms of co-crystal and thereof. Thus, it was suggested that careful attentions is needed during the screening since the co-crystal formation is currently one of the promising approach to be considered in research and development for pharmaceutical industry to improve the poorly soluble drugs.

Structural and Optical Properties of Pr3+ Doped ZnO and PVA:Zn98Pr2O Nanocomposite Free Standing Film

In this work, we report, a systematic study on the structural and optical properties of Pr-doped ZnO nanostructures and PVA:Zn98Pr2O polymer matrix nanocomposites free standing films. These particles are synthesized through simple wet chemical route and solution casting technique at room temperature, respectively. Structural studies carried out by X-ray diffraction method confirm that the prepared pure ZnO and Pr doped ZnO nanostructures are in hexagonal wurtzite structure and the microstrain is increased upon doping. TEM analysis reveals that the prepared materials are in sheet like nature. Absorption spectra show free excitonic absorption band at 370 nm and red shift for the Pr doped ZnO nanostructures. The PVA:Zn98Pr2O composite film exhibits both free excitonic and PVA absorption bands at 282 nm. Fourier transform infrared spectral studies confirm the presence of A1 (TO) and E1 (TO) modes of Zn-O bond vibration and the formation of polymer composite materials.

Control of Airborne Aromatic Hydrocarbons over TiO2-Carbon Nanotube Composites

Poly vinyl acetate (PVA)-based titania (TiO2)–carbon nanotube composite nanofibers (PVA-TCCNs) with various PVA-to-solvent ratios and PVA-based TiO2 composite nanofibers (PVA-TN) were synthesized using an electrospinning process, followed by thermal treatment. The photocatalytic activities of these nanofibers in the degradation of airborne monocyclic aromatics under visible-light irradiation were examined. This study focuses on the application of these photocatalysts to the degradation of the target compounds at sub-part-per-million indoor air concentrations. The characteristics of the photocatalysts were examined using scanning electron microscopy, X-ray diffraction, ultraviolet-visible spectroscopy, and Fourier-transform infrared spectroscopy. For all the target compounds, the PVA-TCCNs showed photocatalytic degradation efficiencies superior to those of the reference PVA-TN. Specifically, the average photocatalytic degradation efficiencies for benzene, toluene, ethyl benzene, and o-xylene (BTEX) obtained using the PVA-TCCNs with a PVA-to-solvent ratio of 0.3 (PVA-TCCN-0.3) were 11%, 59%, 89%, and 92%, respectively, whereas those observed using PVA-TNs were 5%, 9%, 28%, and 32%, respectively. PVA-TCCN-0.3 displayed the highest photocatalytic degradation efficiency for BTEX, suggesting the presence of an optimal PVA-to-solvent ratio for the synthesis of PVA-TCCNs. The average photocatalytic efficiencies for BTEX decreased from 11% to 4%, 59% to 18%, 89% to 37%, and 92% to 53%, respectively, when the flow rate was increased from 1.0 to 4.0 L min1. In addition, the average photocatalytic efficiencies for BTEX increased 11% to ~0%, 59% to 3%, 89% to 7%, and 92% to 13%, respectively, when the input concentration increased from 0.1 to 1.0 ppm. The prepared PVA-TCCNs were effective for the purification of airborne aromatics at indoor concentration levels, particularly when the operating conditions were optimized.

Nanostructured Pt/MnO2 Catalysts and Their Performance for Oxygen Reduction Reaction in Air Cathode Microbial Fuel Cell

Microbial fuel cells (MFCs) represent a promising technology for simultaneous bioelectricity generation and wastewater treatment. Catalysts are significant portions of the cost of microbial fuel cell cathodes. Many materials have been tested as aqueous cathodes, but air-cathodes are needed to avoid energy demands for water aeration. The sluggish oxygen reduction reaction (ORR) rate at air cathode necessitates efficient electrocatalyst such as carbon supported platinum catalyst (Pt/C) which is very costly. Manganese oxide (MnO2) was a representative metal oxide which has been studied as a promising alternative electrocatalyst for ORR and has been tested in air-cathode MFCs. However the single MnO2 has poor electric conductivity and low stability. In the present work, the MnO2 catalyst has been modified by doping Pt nanoparticle. The goal of the work was to improve the performance of the MFC with minimum Pt loading. MnO2 and Pt nanoparticles were prepared by hydrothermal and sol gel methods, respectively. Wet impregnation method was used to synthesize Pt/MnO2 catalyst. The catalysts were further used as cathode catalysts in air-cathode cubic MFCs, in which anaerobic sludge was inoculated as biocatalysts and palm oil mill effluent (POME) was used as the substrate in the anode chamber. The asprepared Pt/MnO2 was characterized comprehensively through field emission scanning electron microscope (FESEM), X-Ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV) where its surface morphology, crystallinity, oxidation state and electrochemical activity were examined, respectively. XPS revealed Mn (IV) oxidation state and Pt (0) nanoparticle metal, indicating the presence of MnO2 and Pt. Morphology of Pt/MnO2 observed from FESEM shows that the doping of Pt did not cause change in needle-like shape of MnO2 which provides large contacting surface area. The electrochemical active area of the Pt/MnO2 catalysts has been increased from 276 to 617 m2/g with the increase in Pt loading from 0.2 to 0.8 wt%. The CV results in O2 saturated neutral Na2SO4 solution showed that MnO2 and Pt/MnO2 catalysts could catalyze ORR with different catalytic activities. MFC with Pt/MnO2 (0.4 wt% Pt) as air cathode catalyst generates a maximum power density of 165 mW/m3, which is higher than that of MFC with MnO2 catalyst (95 mW/m3). The open circuit voltage (OCV) of the MFC operated with MnO2 cathode gradually decreased during 14 days of operation, whereas the MFC with Pt/MnO2 cathode remained almost constant throughout the operation suggesting the higher stability of the Pt/MnO2 catalyst. Therefore, Pt/MnO2 with 0.4 wt% Pt successfully demonstrated as an efficient and low cost electrocatalyst for ORR in air cathode MFC with higher electrochemical activity, stability and hence enhanced performance.

New Method for Determining the Distribution of Birefringence and Linear Dichroism in Polymer Materials Based On Polarization-Holographic Grating

A new method for determining the distribution of birefringence and linear dichroism in optical polymer materials is presented. The method is based on the use of polarizationholographic diffraction grating that forms an orthogonal circular basis in the process of diffraction of probing laser beam on the grating. The intensities ratio of the orders of diffraction on this grating enables the value of birefringence and linear dichroism in the sample to be determined. The distribution of birefringence in the sample is determined by scanning with a circularly polarized beam with a wavelength far from the absorption band of the material. If the scanning is carried out by probing beam with the wavelength near to a maximum of the absorption band of the chromophore then the distribution of linear dichroism can be determined. An appropriate theoretical model of this method is presented. A laboratory setup was created for the proposed method. An optical scheme of the laboratory setup is presented. The results of measurement in polymer films with two-dimensional gradient distribution of birefringence and linear dichroism are discussed.

Formulation and ex vivo Evaluation of Solid Lipid Nanoparticles (SLNS) Based Hydrogel for Intranasal Drug Delivery

Risperidone (RISP) is an antipsychotic agent and has low water solubility and nontargeted delivery results in numerous side effects. Hence, an attempt was made to develop SLNs hydrogel for intranasal delivery of RISP to achieve maximum bioavailability and reduction of side effects. RISP loaded SLNs composed of 1.65% (w/v) lipid mass were produced by high shear homogenization (HSH) coupled ultrasound (US) method using glycerylmonostearate (GMS) or Imwitor 900K (solid lipid). The particles were loaded with 0.2% (w/v) of the RISP & surface-tailored with a 2.02% (w/v) non-ionic surfactant Tween® 80. Optimization was done using 32 factorial design using Design Expert® software. The prepared SLNs dispersion incorporated into Polycarbophil AA1 hydrogel (0.5% w/v). The final gel formulation was evaluated for entrapment efficiency, particle size, rheological properties, X ray diffraction, in vitro diffusion, ex vivo permeation using sheep nasal mucosa and histopathological studies for nasocilliary toxicity. The entrapment efficiency of optimized SLNs was found to be 76 ± 2%, polydispersity index