Anthocyanin Complex: Characterization and Cytotoxicity Studies

Complexation of anthocyanins to mimic natural copigmentation process was investigated. Cyanidin-rich extracts from Zea mays L. ceritina Kulesh. and delphinidin-rich extracts from Clitoria ternatea L. 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.

Acid Fuchsin Dye Based PMMA Film for Holographic Investigations

In view of a possible application in optical data storage devices, diffraction grating efficiency of an organic dye, Acid Fuchsin doped in PMMA matrix was studied under excitation with CW diode pumped Nd: YAG laser at 532 nm. The open aperture Zscan of dye doped polymer displayed saturable absorption and the closed aperture Z-scan of the samples exhibited negative nonlinearity. The diffraction efficiency of the grating is the ratio of the intensity of the first order diffracted power to the incident read beam power. The dye doped polymer films were found to be good media for recording. It is observed that the formation of gratings strongly depend on the concentration of dye in the polymer film, the intensity ratios of the writing beams and the angle between the writing beams. It has been found that efficient writing can be made at an angle of 20o and when the intensity ratio of the writing beams is unity.

Investigation of VN/TiN Multilayer Coatings on AZ91D Mg Alloys

To develop AZ91D magnesium alloys with improved properties, we have applied TiN and VN/TiN multilayer coatings using DC magnetron sputter technique. Coating structure, surface morphology, chemical bonding and corrosion resistance of coatings were analyzed by x-ray diffraction (XRD), scanning electron microscope (SEM), x-ray photoelectron spectroscopy (XPS), and tafel extrapolation method, respectively. XPS analysis reveal that VN overlayer reacts with oxygen at the VN/TiN interface and forms more stable TiN layer. Morphological investigations and the corrosion results show that VN/TiN multilayer thin film coatings are quite effective to optimize the corrosion resistance of Mg alloys.

Gas-Solid Nitrocarburizing of Steels: Kinetic Modeling and Experimental Validation

The study is devoted to define the optimal conditions for the nitriding of pure iron at atmospheric pressure by using NH3- Ar-C3H8 gas mixtures. After studying the mechanisms of phase formation and mass transfer at the gas-solid interface, a mathematical model is developed in order to predict the nitrogen transfer rate in the solid, the ε-carbonitride layer growth rate and the nitrogen and carbon concentration profiles. In order to validate the model and to show its possibilities, it is compared with thermogravimetric experiments, analyses and metallurgical observations (X-ray diffraction, optical microscopy and electron microprobe analysis). Results obtained allow us to demonstrate the sound correlation between the experimental results and the theoretical predictions.

Microcrystalline Cellulose (MCC) From Oil Palm Empty Fruit Bunch (EFB) Fiber via Simultaneous Ultrasonic and Alkali Treatment

In this study, microcrystalline cellulose (MCC) was extracted from oil palm empty fruit bunch (EFB) cellulose which was earlier isolated from oil palm EFB fibre. In order to isolate the cellulose, the chlorination method was carried out. Then, the MCC was prepared by simultaneous ultrasonic and alkali treatment from the isolated α-cellulose. Based on mass balance calculation, the yields for MCC obtained from EFB was 44%. For fiber characterization, it is observed that the chemical composition of the hemicellulose and lignin for all samples decreased while composition for cellulose increased. The structural property of the MCC was studied by X-ray diffraction (XRD) method and the result shows that the MCC produced is a cellulose-I polymorph, with 73% crystallinity.

Preparation and Fabrication of Lithium Disilicate Glass Ceramic as Dental Crowns via Hot Pressing Method

Two Lithium Disilicate (LD) glass ceramics based on SiO2-Li2O-K2O-Al2O3 system were prepared through a glass melting method. The glass rods were then fabricated into dental crowns via a hot pressing at 900˚C and 850˚C in order to study the effect of the pressing temperatures on the phase formation and microstructure of the glasses. Different samples of as cast glass and heat treated samples (600˚C and 700˚C) were used to press for investigating the effect of an initial microstructure on the hot pressing technique. Xray diffraction (XRD) and scanning electron microscopy (SEM) were performed to determine the phase formation and microstructure of the samples, respectively. XRD results show that the main crystalline structure was Li2Si2O5 by having Li3PO4, Li0.6Al0.6Si2O6, Li2SiO3, Ca5 (PO4)3F and SiO2 as minor phases. Glass compositions with different heat treatment temperatures exhibited a difference phase formations but have less effect during pressing. SEM micrographs showed the microstructure of Li2Si2O5 as lath-like shape in all glasses. With increasing the initial heat treatment temperature, the longer the lath-like crystals of lithium disilicate were increased especially when using glass heat treatment at 700˚C followed by pressing at 900˚C. This could be suggested that LD1 heat treatment at 700˚C which pressing at 900˚C presented the best formation by the hot pressing and compiled microstructure.

Synthesis of Y2O3 Films by Spray Coating with Milled EDTA·Y·H Complexes

Yttrium oxide (Y2O3) films have been successfully deposited with yttrium-ethylenediamine tetraacetic acid (EDTA·Y·H) complexes prepared by various milling techniques. The effects of the properties of the EDTA·Y·H complex on the properties of the deposited Y2O3 films have been analyzed. Seven different types of the raw EDTA·Y·H complexes were prepared by various commercial milling techniques such as ball milling, hammer milling, commercial milling, and mortar milling. The milled EDTA·Y·H complexes exhibited various particle sizes and distributions, depending on the milling method. Furthermore, we analyzed the crystal structure, morphology and elemental distribution profile of the metal oxide films deposited on stainless steel substrate with the milled EDTA·Y·H complexes. Depending on the milling technique, the flow properties of the raw powders differed. The X-ray diffraction pattern of all the samples revealed the formation of Y2O3 crystalline phase, irrespective of the milling technique. Of all the different milling techniques, the hammer milling technique is considered suitable for fabricating dense Y2O3 films.

In-situ Observations Using SEM-EBSD for Bending Deformation in Single-Crystal Materials

To elucidate the material characteristics of single crystals of pure aluminum and copper, the respective relations between crystallographic orientations and microstructures were examined, along with bending and mechanical properties. The texture distribution was also analysed. Bending tests were performed in a SEM apparatus while its behaviors were observed. Some analytical results related to crystal direction maps, inverse pole figures, and textures were obtained from electron backscatter diffraction (EBSD) analyses.

The Interaction between Hydrogen and Surface Stress in Stainless Steel

This paper reveals the interaction between hydrogen and surface stress in austenitic stainless steel by X-ray diffraction stress measurement and thermal desorption analysis before and after being charged with hydrogen. The surface residual stress was varied by surface finishing using several disc polishing agents. The obtained results show that the residual stress near surface had a significant effect on hydrogen absorption behavior, that is, tensile residual stress promoted the hydrogen absorption and compressive one did opposite. Also, hydrogen induced equi-biaxial stress and this stress has a linear correlation with hydrogen content.

Preparation and Characterization of Calcium Phosphate Cement

Calcium phosphate cement (CPC) is one of the most attractive bioceramics due to its moldable and shape ability to fill complicated bony cavities or small dental defect positions. In this study, CPC was produced by using mixture of tetracalcium phosphate (TTCP, Ca4O(PO4)2) and dicalcium phosphate anhydrous (DCPA, CaHPO4) in equimolar ratio (1/1) with aqueous solutions of acetic acid (C2H4O2) and disodium hydrogen phosphate dehydrate (Na2HPO4.2H2O) in combination with sodium alginate in order to improve theirs moldable characteristic. The concentration of the aqueous solutions and sodium alginate were varied to investigate the effect of different aqueous solutions and alginate on properties of the cements. The cement paste was prepared by mixing cement powder (P) with aqueous solution (L) in a P/L ratio of 1.0g/0.35ml. X-ray diffraction (XRD) was used to analyses phase formation of the cements. Setting time and compressive strength of the set CPCs were measured using the Gilmore apparatus and Universal testing machine, respectively. The results showed that CPCs could be produced by using both basic (Na2HPO4.2H2O) and acidic (C2H4O2) solutions. XRD results show the precipitation of hydroxyapatite in all cement samples. No change in phase formation among cements using difference concentrations of Na2HPO4.2H2O solutions. With increasing concentration of acidic solutions, samples obtained less hydroxyapatite with a high dicalcium phosphate dehydrate leaded to a shorter setting time. Samples with sodium alginate exhibited higher crystallization of hydroxyapatite than that of without alginate as a result of shorten setting time in a basic solution but a longer setting time in an acidic solution. The stronger cement was attained from samples using the acidic solution with sodium alginate; however the strength was lower than that of using the basic solution.

Mercury Removing Capacity of Multiwall Carbon Nanotubes as Detected by Cold Vapor Atomic Absorption Spectroscopy: Kinetic & Equilibrium Studies

Multiwall carbon nanotubes, prepared by chemical vapor deposition, have an average diameter of 60-100 nm as shown by High Resolution Transmittance Electron Microscope, HR-TEM. The Multiwall carbon nanotubes (MWCNTs) were further characterized using X-ray Diffraction and Raman Spectroscopy. Mercury uptake capacity of MWCNTs was studied using batch adsorption method at different concentration ranges up to 150 ppm. Mercury concentration (before and after the treatment) was measured using cold vapor atomic absorption spectroscopy. The effect of time, concentration, pH and adsorbent dose were studied. MWCNT were found to perform complete absorption in the sub-ppm concentrations (parts per billion levels) while for high concentrations, the adsorption efficiency was 92% at the optimum conditions; 0.1 g of the adsorbent at 150 ppm mercury (II) solution. The adsorption of mercury on MWCNTs was found to follow the Freundlich adsorption isotherm and the pseudo-second order kinetic model.

The Effect of Impinging WC-12Co Particles Temperature on Thickness of HVOF Thermally Sprayed Coatings

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

High-Temperature X-Ray Powder Diffraction of Secondary Gypsum

This paper involved the performance of a hightemperature X-Ray powder diffraction analysis (XRD) of a sample of chemical gypsum generated in the production of titanium white; this gypsum originates by neutralizing highly acidic water with limestone suspension. Specifically, it was gypsum formed in the first stage of neutralization when the resulting material contains, apart from gypsum, a number of waste products resulting from the decomposition of ilmenite by sulphuric acid. So it can be described as red titanogypsum. By conducting the experiment using XRD apparatus Bruker D8 Advance with a Cu anode (λkα=1.54184 Å) equipped with high-temperature chamber Anton Paar HTK 16, it was possible to identify clearly in the sample each phase transition in the system of CaSO4·xH2O.

Effects of Additives on Thermal Decompositions of Carbon Black/High Density Polyethylene Compounds

In the present work, the effects of additives, including contents of the added antioxidants and type of the selected metallic stearates (either calcium stearate (CaSt) or zinc stearate (ZnSt)), on the thermal stabilities of carbon black (CB)/high density polyethylene (HDPE) compounds were studied. The results showed that the AO contents played a key role in the thermal stabilities of the CB/HDPE compounds — the higher the AO content, the higher the thermal stabilities. Although the CaSt-containing compounds were slightly superior to those with ZnSt in terms of the thermal stabilities, the remaining solid residue of CaSt after heated to the temperature of 600 °C (mainly calcium carbonate (CaCO3) as characterized by the X-ray diffraction (XRD) technique) seemed to catalyze the decomposition of CB in the HDPE-based compounds. Hence, the quantification of CB in the CaSt-containing compounds with a muffle furnace gave an inaccurate CB content — much lower than actual value. However, this phenomenon was negligible in the ZnSt-containing system.

Stabilization of Transition Metal Chromite Nanoparticles in Silica Matrix

This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nanocrystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nanocomposites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900−1200 ◦C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nanocrystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ∼4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nanoparticles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nanocrystals were found to be just moderately modified in comparison to the bulk phases.

Enhancing Protein Incorporation in Calcium Phosphate Coating on Titanium by Rapid Biomimetic Co-Precipitation Technique

Calcium phosphate coating (CaP) has been employed for protein delivery, but the typical direct protein adsorption on the coating led to low incorporation content and fast release of the protein from the coating. By using bovine serum albumin (BSA) as a model protein, rapid biomimetic co-precipitation between calcium phosphate and BSA was employed to control the distribution of BSA within calcium phosphate coating during biomimetic formation on titanium surface for only 6 h at 50oC in an accelerated calcium phosphate solution. As a result, the amount of BSA incorporation and release duration could be increased by using a rapid biomimetic coprecipitation technique. Up to 43 fold increases in the BSA incorporation content and the increase from 6 h to more than 360 h in release duration compared to typical direct adsorption technique were observed depending on the initial BSA concentration used during coprecipitation (1, 10 and 100 μg.ml-1). From x-ray diffraction and Fourier transform infrared spectroscopy studies, the coating composition was not altered with the incorporation of BSA by this rapid biomimetic co-precipitation and mainly comprised octacalcium phosphate and hydroxyapatite. However, the microstructure of calcium phosphate crystals changed from straight, plate-like units to curved, plate-like units with increasing BSA content.

Conversion of Jatropha curcas Oil to Ester Biolubricant Using Solid Catalyst Derived from Saltwater Clam Shell Waste (SCSW)

The discarded clam shell waste, fossil and edible oil as biolubricant feedstocks create environmental impacts and food chain dilemma, thus this work aims to circumvent these issues by using activated saltwater clam shell waste (SCSW) as solid catalyst for conversion of Jatropha curcas oil as non-edible sources to ester biolubricant. The characterization of solid catalyst was done by Differential Thermal Analysis-Thermo Gravimetric Analysis (DTATGA), X-Ray Fluorescence (XRF), X-Ray Diffraction (XRD), Brunauer-Emmett-Teller (BET), Field Emission Scanning Electron Microscopy (FESEM) and Fourier Transformed Infrared Spectroscopy (FTIR) analysis. The calcined catalyst was used in the transesterification of Jatropha oil to methyl ester as the first step, and the second stage was involved the reaction of Jatropha methyl ester (JME) with trimethylolpropane (TMP) based on the various process parameters. The formated biolubricant was analyzed using the capillary column (DB-5HT) equipped Gas Chromatography (GC). The conversion results of Jatropha oil to ester biolubricant can be found nearly 96.66%, and the maximum distribution composition mainly contains 72.3% of triester (TE).

Magnetic Properties of Sr-Ferrite Nano-Powder Synthesized by Sol-Gel Auto-Combustion Method

In this paper, strontium ferrite (SrO.6Fe2O3) was synthesized by the sol-gel auto-combustion process. The thermal behavior of powder obtained from self-propagating combustion of initial gel was evaluated by simultaneous differential thermal analysis (DTA) and thermo gravimetric (TG), from room temperature to 1200°C. The as-burnt powder was calcined at various temperatures from 700-900°C to achieve the single-phase Sr-ferrite. Phase composition, morphology and magnetic properties were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. Results showed that the single-phase and nano-sized hexagonal strontium ferrite particles were formed at calcination temperature of 800°C with crystallite size of 27 nm and coercivity of 6238 Oe.

Mechanical Properties of 3D Noninterlaced Cf/SiC Composites Prepared through Hybrid Process (CVI+PIP)

Three dimensional non-Interlaced carbon fibre reinforced silicon carbide (3-D-Cf/SiC) composites with pyrocarbon interphase were fabricated using isothermal chemical vapor infiltration (ICVI) combined with polymer impregnation pyrolysis (PIP) process. Polysilazane (PSZ) is used as a preceramic polymer to obtain silicon carbide matrix. Thermo gravimetric analysis (TGA), Infrared spectroscopic analysis (IR) and X-ray diffraction (XRD) analysis were carried out on PSZ pyrolysed at different temperatures to understand the pyrolysis and obtaining the optimum pyrolysing condition to yield β-SiC phase. The density of the composites was 1.94 g cm-3 after the 3-D carbon preform was SiC infiltrated for 280 h with one intermediate polysilazane pre-ceramic PIP process. Mechanical properties of the composite materials were investigated under tensile, flexural, shear and impact loading. The values of tensile strength were 200 MPa at room temperature (RT) and 195 MPa at 500°C in air. The average RT flexural strength was 243 MPa. The lower flexural strength of these composites is because of the porosity. The fracture toughness obtained from single edge notched beam (SENB) technique was 39 MPa.m1/2. The work of fracture obtained from the load-displacement curve of SENB test was 22.8 kJ.m-2. The composites exhibited excellent impact resistance and the dynamic fracture toughness of 44.8 kJ.m-2 is achieved as determined from instrumented Charpy impact test. The shear strength of the composite was 93 MPa, which is significantly higher compared 2-D Cf/SiC composites. Microstructure evaluation of fracture surfaces revealed the signatures of fracture processes and showed good support for the higher toughness obtained.

An Investigation of New Phase Diagram of Ag2SO4 - CaSO4

A phase diagram of the Ag2SO4 - CaSO4 (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag2SO4 + CaSO4) is observed at 10 mole% CaSO4 and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca 2+ in Ag2SO4 is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO4 content. Amongst other binary compositions, the 80AgSO4-20CaSO4 gave improved sinterability/packing density.