Monoclinic bismuth oxide (α-Bi2O3) nanoparticles were prepared via precipitation method and
irradiated with a pulsed laser forming thin films. Their phase and surface morphological properties
were investigated using x-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron
microscopy (SEM) and high resolution transmission electron microscopy (HR-TEM). The XRD
analysis shows the phase transformation to a partially crystalline tetragonal phase β-Bi2O3 thin film.
The SEM micrograph of the nanoparticles, with an average crystal size of 72 nm, was seen to form
a thin film with a peculiar structure, coined as “cotton-like”, is attributed to the high surface energy
absorbed by the nanoparticles during ablation. The HR-TEM micrograph shows the particulate with
a clearly defined interlayer spacing.
Titanium alloy (e.g. Ti-6Al-4V) has an excellent combination of properties. However in many cases,
the application is limited because of the poor wear property. In this work, a surface modification
(plasma nitriding) is carried out to improve the surface properties of Ti-6Al-4V, as a treatment prior to a hardcoating deposition, leading to a duplex coating system. This is an effort to improve the surface and near surface property of Ti-6Al-4V. Plasma nitriding is performed utilizing microwave plasma method in 25% Ar- 75% N2 atmosphere at temperatures of 600°C and 700°C for different processing times (1, 3 and 5 hours). The phase and microstructure of plasma nitrided substrate were characterized by using X-ray diffraction (XRD) and Scanning electron microscopy (SEM). The plasma nitrided Ti-6Al-4V properties (surface roughness, surface hardness and case depth) were determined using profilometer and microhardness, respectively. Results obtained showed a significant increase on the surface hardness of Ti-6Al-4V. This is due to the formation of TiN and Ti2N phases in the form of compound layer. Besides, it shows that the diffusion of nitrogen into the Ti-6Al-4V substrate produces case depth up to 130 µm and this contributes to the improvement of the near surface hardness due to the changes in the microstructures. It was also found that the surface hardness and surface roughness increased with the increases in the process temperature and times.
Bismuth chromium solid solutions, with a general formula Bi6-xCr2Oδ, where -1 ≤ x ≤ 2, were successfully synthesized via the conventional solid state method. The phases of the synthesized samples were determined by X-ray diffraction (XRD) analysis. The properties of single-phase compounds were characterized by using differential thermal analysis (DTA), thermal gravimetric analysis (TGA), AC impedance spectroscopy, and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The occurrence of phase transitions was confirmed by DTA and TGA, where a thermal event was observed by DTA at around 800oC. In addition, TGA studies also showed that there was a weight loss at around 800oC. Elemental analysis of Bi6Cr2O15 and its solid solutions by ICP-AES showed a good agreement between the expected value and the experimental value on the compositions, with no evidence of any systematic deviation from stoichiometric. Electrical properties of Bi6Cr2O15 and its solid solutions were investigated by using AC impedance spectroscopy from 300oC to 650oC. Ionic conductivity increased with the increasing temperature and bismuth content, and the best ionic conductivity was observed for Bi7Cr2O16.5. The activation energy (Ea) of Bi6Cr2O15 and its solid solutions were in the range of 1.22-1.32 eV.
Ordered microporous NaY zeolite and mesoporous copper oxide are high performance material as catalysts and adsorbents. The copper oxide-NaY zeolite modification in combination of their physicochemical properties could provide excellent opportunities for the creation of new gas adsorbents. In this study, modified NaY zeolite properties and methane adsorptive characteristics were investigated by dispersing copper oxide onto the NaY zeolite structure using the thermal dispersion method. The structures of the copper oxide modified zeolites were characterized by powder X-ray diffraction and Micromeritics ASAP 2000, while the methane adsorption characteristics were analyzed using a thermogravimetric analyzer. The results revealed that types of copper oxide, copper oxide loading concentration, calcination temperature and calcination time greatly affected the modified zeolite structure and gas methane adsorption characteristics.
Among the challenges for superconducting devices to be applied in industry are the need for high transport critical current density (Jr) and sustainability of the device in different environment. For superconducting material to maintain high 4, effective flux pinning centers are needed. The addition of small size MgO particles in bulk Bi2Sr2CaCu2O8 (Bi-2212) superconductor has been proven to enhance the effective flux pinning centers in the superconducting material. Nevertheless, the flux pinning properties of the superconducting materials may change if they are exposed to radioactive environment. Electron irradiation is one of the common techniques that can be used to study the impact of irradiation on superconducting materials. In this work, a small amount of nanosize MgO particles were used as the flux pinning centers for Bi-2212 superconducting material. The Bi-2212/MgO composite was heat treated and followed by partial melting and slow cooling. Some of the samples were subjected to electron irradiation using the facility at the Malaysian Nuclear Agency. Characterizations of non-irradiated and irradiated samples were performed via X-ray Diffraction Patterns (XRD), Scanning Electron Microscopy (SEM) and measurements of J, dependence on temperature in self-field. Higher J, indicates better flux pinning properties in irradiated superconductor composite. This is achieved if defects with larger radius with dimension comparable to the coherence length of the superconducting material were created. On the other hand, decreased in Je indicates ineffective flux pinning and this is attributed to the overlapping of defects that break the superconducting region. Our study showed that electron irradiation deteriorated the flux pinning properties of the Bi-2212/MgO superconductor composite.
Anion clay hydrotalcite MgA1C0 3 with a Mg/A1 molar ratio of 3:1 was synthesized by co-precipitation at room temperature and pressure. The physicochemical properties were evaluated using Powder X-Ray Diffraction (PXRD), Fourier Transform Infrared (FTIR) spectroscopy and Thermogravimetric Analysis (TGA). The efficacy of anion clay hydrotalcite in the removal ofCcf- from aqueous solutions was investigated with respect to contact time, initial concentration, pH, adsorbent dosage and temperature. The Cd2- removal increased with the increased in contact time, adsorbent dosage, pH and initial concentration. Adsorption decreases with increasing initial concentration and temperature, for which the latter is indicative of an exothermic process. The equilibrium adsorption capacity of MgA1C0 3 was evaluated using linear Langmuir and Freundlich isotherms with respect to the separation factor, RL.
Al-Si/SiC composites with the fraction of 5 and 15 wt. % fine SiC particles were fabricated using stir casting process by which SiC powders were poured into aluminium melt and cast in a stainless steel mould to form ingot. Characterization by X-ray diffraction (XRD) analysis showed the presence of constituent and intermetallic materials in the composites. Microstructure study revealed that both fine and course particles scattered in the Al-Si matrix. The characterization of thermal properties showed that the thermal conductivity and coefficient of thermal expansion decreased with the increase in SiC content. The conductivity and expansion behavior is correlated to the microstructure and weight fraction of the SiC particles. Meanwhile, the hardness of the composite increased with the increasing of SiC particles in the composites.
The term microfibril angle, MFA in wood science refers to the angle between the direction of the helical windings of cellulose microfibrils in the secondary cell wall, S2 layer of fibres and tracheids and the long axis of the cell. In this study, the mean MFA of the cell walls were determined for thin samples of thickness 200.0 µm from pith and outwards, for eight ages of Acacia mangium wood. The determination of MFA was based on a diffraction pattern arising from cellulose crystal planes of the type 002 generated by x-ray diffraction and recorded using an electronic detector. The results show an inversely relationship between MFA and age of tree in Acacia mangium wood. MFA decreased from 26.13° at age 3 year-old to 0.20° at tree of age 15 year-old for the pith region. The most significant drop occurred from 16.14° at age 7 yearold to 11.30° at age 9 year-old. An inversely relationship between MFA and storage modulus E’ was evidence in Acacia mangium at age 10-year-old. The results showed that about 76.22% variation of loss modulus E” was attributed to the MFA, while about 66.4% of the variation of glass transition Tg was explained by MFA under the same experimental conditions.
Silicon nanowires were synthesized on Si substrates (111) via thermal evaporation using AuPd thin layer catalyst. Pre cleaned of Si wafer was used as a substrate to assemble the nanostructure products. In this work, the effect of growth temperature that ranging from 800 to 1000°C on the formation of silicon nanowires studied extensively. X-ray diffraction and field emission scanning electron microscope were employed to characterize the structures and morphology of nanowires. Vertical aligned silicon nanowires have been successfully grown on Si substrates at 900 and 1000°C. At 1100°C, the high aspect ratio of silicon nanowires can be produced but the formation density is low. The presence of AuPd catalyst on the tip of nanowires, it is expected that VLS is the most suitable to explain the growth mechanism of obtained SiNWs. The crystalline structure of SiNWs was proved by XRD data.
Herein, we report on the optimum condition for TiO2, titania nanotubes formation and the effect of annealing on the formation of anatase and rutile titania. Anodic oxidation was carried out in two electrodes bath consisting of 5wt% NH4F ions. The anode was a 0.1mm thick Ti foil and the cathode was Pt electrode. Anodisation was conducted at 20V. The anodised foils were subjected to morphological and structural characterizations. As-anodised foil was found to be amorphous or weakly crystalline. When the oxide was heat treated, x-ray diffraction analysis revealed the presence of (101) anatase at annealing temperature from 400-500°C. This indicates that the transformation occurs at this range of temperatures. Raman spectroscopy analysis showed the diminishing of anatase peaks for samples annealed at 500°C. At above 600°C, x-ray diffraction pattern shows a peak belonging to the rutile peak. Transformation from anatase to rutile is thought to occur at about 500°C with a more complete transformation at higher temperature. Annealing at higher than 600°C induces thickening of the nanotubes wall and at above 700°C, the nanotubes structure has completely disappeared.
Production of carbon dioxide from degraded woods especially Karas or Aquilariella Malaccensis using integrated pyrolysis-combustion is important for radiocarbon dating application. The effects of pyrolysis temperatures (300-400 0 C), retention times (20-35 minutes) and flow rates of argon (400- 1000 ml/min) on the production of carbon dioxide were studied. The experiments were arranged according to a 2 3 response surface central composite statistical design (CSD). This response surface methodology (RSM) was used to assess factor interactions and empirical models regarding carbon dioxide yield. The optimized yield of carbon dioxide was 82.57% for Karas and the optimum reaction conditions are 300 0 C of pyrolysis temperature, 20 minutes retention time and 982ml/min flow rates of argon. Scanning electron microscope (SEM) and X-ray Diffraction (XRD) were conducted to assess the morphological characteristics of the woods and to look at the potential crystalline structure produced after the process took place, respectively.
Clay has been regarded as very important natural industrial materials. All these industries exploit the properties that clay can be molded into any shape and fired to dry without losing its form. A study was carried out on clay samples from eight sites in the north-eastern part of Peninsular Malaysia. The study was accomplished by using X-ray diffraction (XRD) technique. The x-ray diffraction spectra obtained enable the determination of the lattice spacing associated with the types of clay and nonclay minerals present in the samples. Results of the study shows that the major components of clay minerals present in all samples studied are kaolinite and illite. The presence of kaolinite is confirmed by firing test in which the kaolinite diffraction peaks disappeared upon heating the samples at 600 o C. The presence of non-clay minerals such as quartz, mica, feldspar and chlorite are also observed.
Synthesis and characterization of supported metal-based oxygen carriers were carried out to provide information related to the use of oxygen carriers for chemical looping combustion processes. The Cu, Co, Fe, Ni metals supported with Al2O3, CeO2, TiO2, ZrO2 were prepared using the wetness impregnation technique. Then, the X-ray Diffraction (XRD) characterization of oxidized and reduced samples was obtained and presented. The kinetic analysis using Thermogravimetric analyzer (TGA) of the synthesized samples was conducted. The kinetics of reduction reaction of all samples were estimated and explained.
Solid polymer electrolyte based on methyl cellulose (MC)-lithium triflate (LiCF3SO3) plasticised with ethylene carbonate (EC) was prepared using solution cast technique. The X-ray diffraction (XRD) studies proved that the amorphous nature of the electrolyte systems was increases due to the addition of salt and plasticiser. The improved surface morphology of plasticised polymer system ensures it has good electrode-electrolyte contact during performance testing. The polymer electrolyte was found to have high thermal stability indicating that the electrolyte can be used at higher temperature. The ionic conductivity increased up to 1.24 x 10-4 S cm-1 at optimum amount of EC plasticiser associated to the effect of plasticiser that initially leads to the formation of Li+-EC complex. Consequently, it reduces the fraction of polymer-Li+ complex which contributes to the increase of the segmental chain flexibility in the plasticized system. Temperature dependent studies indicate ionic conductivity increase due to the temperature increase and is in line with Arrhenius behaviour pattern. An activation energy of 0.26 eV at highest conductivity sample was obtained. The addition of plasticiser lowers the activation energy thus increasing the ion mobility of the system and contributing to ionic conductivity increment. The plasticization method is a promising means to dealing with the solid polymer electrolyte problem and producing electrolytes that meet the needs of electrochemical devices.
ZnO with two different morphologies were used to study the inhibition of Streptococcus sobrinus and Streptococcus mutans which are closely associated with tooth cavity. Rod-like shaped ZnO-A and plate-like shaped ZnO-B were produced using a zinc boiling furnace. The nanopowders were characterized using energy filtered transmission electron microscopy (EFTEM), X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, Raman spectroscopy and dynamic light scattering (DLS) to confirm the properties of the ZnO polycrystalline wurtzite structures. XRD results show that the calculated crystallite sizes of ZnO-A and ZnO-B were 36.6 and 39.4nm, respectively, whereas DLS revealed particle size distributions of 21.82nm (ZnO-A) and 52.21nm (ZnO-B). PL spectra showed ion vacancy defects related to green and red luminescence for both ZnO particles. These defects evolved during the generation of reactive oxygen species which contributed to the antibacterial activity. Antibacterial activity was investigated using microdilution technique towards S. sobrinus and S. mutans at different nanopowder concentrations. Results showed that ZnO-A exhibited higher inhibition on both bacteria compared with ZnO-B. Moreover, S. mutans was more sensitive compared with S. sobrinus because of its higher inhibition rate.
Glass-ceramics are a group of materials that takes advantage of the various glass-forming methods before they are subsequently heat-treated in a controlled manner to effect nucleation and crystallization to produce crystalline materials. The production of glassceramic materials is to overcome the low mechanical strength in pure glassy materials. In this work, a study on the crystallisation of a soda-lime-silica glass was undertaken to ascertain how the processing parameters affect the crystallization of such glasses, viz. either via a single or two-step heat-treatment procedure, as well as the effect of soaking duration at the heat-treatment temperature. A soda-lime-silica glass system was chosen because the raw materials for producing such glasses are readily available and can be considered to be the cheapest. The glass produced was examined by thermal analysis to determine the nucleation and crystallization temperatures before they were heat-treated using a single-step and a two-stage heat-treatment procedures. The resultant glassceramics produced were characterized using x-ray diffraction as well as by scanning electron microscopy. The results thus obtained showed that a two-stage heat-treatment procedure is more successful in producing a well-crystallized glass-ceramic product.
Various techniques are commonly used to produce nano-crystalline NiAl2O4 materials; however, their practical applications in the microwave region remain very limited. In this work, flexible substrates for metamaterials containing two different concentrations of NiAl2O4 (labelled Ni36 and Ni42) have been synthesised using a sol-gel method. The formation of spinel structures in the synthesised materials is confirmed, and their crystalline sizes are determined using scanning electron microscopy, X-ray diffraction, and energy dispersive X-ray techniques. The dielectric properties, conductivities, loss tangents, and other parameters of the NiAl2O4-based substrates are analysed to evaluate their applicability as dielectric materials for the microwave frequency range. The obtained results show that the fabricated Ni36 and Ni42 nickel aluminates possess dielectric constants of 4.94 and 4.97 and loss tangents of 0.01 and 0.007, respectively; in addition, they exhibit high flexibility and light weight, which make them suitable for applications as metamaterial substrates. The synthesised structures are also validated experimentally using a commercially available electromagnetic simulator; as a result, double negative behaviour of the flexible metamaterials has been observed. Furthermore, it is found that the prepared NiAl2O4 substrates can be used in the S-, C-, and X-bands of the microwave frequency region.
Corrosion caused by sulphate-reducing bacteria (SRB) isolated from seawater nearby to Pasir Gudang has been studied. The test coupon was a AISI 304 stainless steel. Potential and corrosion rate measurements were carried out in various types of culturing solutions, with SRB1, SRB2, combination of SRB1 & SRB2 and without SRBs inoculated (sterilized). From Tafel plots a higher corrosion rate has been found in medium inoculated with SRBs than that of the sterilized medium (control). When SRBs were present in the medium, the Tafel plot shifted towards more negative values (Ecorr was shifted to much less anodic values) and increase in current density compared to that of the sterilized medium (control). Localized corrosion was observed on the metal surface, and it was associated to the SRB activity. X-ray analysis (EDAX) showed that the corrosion product has higher content of sulphur for medium containing SRBs than that of the sterilized medium. X-Ray Diffraction analysis carried out on corrosion products which showed the presence of iron sulphide. This indicates the influence of the presence of SRB in corrosion process.
Titanium dioxide particles were successfully prepared using microemulsion-mediated hydrothermal processing route, with sucrose ester as a stabilising agent. X-ray diffraction patterns revealed that the particles possessed anatase crystal phase. Scanning electron micrographs showed micron-sized spherical particles with rough and smooth surfaces, which eventually interconnected with one another. The formation mechanism of the titanium dioxide microstructures was postulated. The as-prepared particles were subjected to photocatalytic degradation of methylene blue, which exhibited higher photocatalytic activity compared to their commercial counterpart.
Nitridation behaviour of Al-Mg-Si alloys was studied as a function of temperature by means of thermogravimetry method. A reactive gas, N2-4%H2 at a rate of 10 ml/min was purged into the thermogravimetry analyser chamber. The Al alloys were heated from 25oC to 625oC at the heating rate of 15oC/min and then reduced to 3oC/min until it reached 1500oC. It was found that by varying the amount of Mg and Si in Al-Mg-Si alloys significantly influenced the growth of the composites. A differential thermogravimetric curve shows the Mg containing alloys experienced many steps of chemical reactions. This indicates that besides AlN presence as a major phase, other compounds also exist in the final product. The X-ray diffraction results confirmed the existence of oxide phases such as a-Al2O3, MgAl2O4 and MgO in addition to residual Si and Al metal. The presence of oxide compounds is believed to be due to the reaction between the alloying elements and residual oxygen gas left in the reaction atmosphere. It was also found that Si could play a role in promoting the weight gain of the composite produced. The heating rate has also a profound effect on the weight gain, whereby higher heating rate resulted in low yielded of AlN during the nitridation reaction of the Al-Mg-Si alloys.