Fine grinding of high purity talc in jet mill at low grinding pressure was carried out by varying the feed rate and classifier rotational speed. These ground particles were sonicated in laboratory ultrasonic bath by varying the soniction period at five levels. The ground and sonicated particles were characterized in terms of particle size and particle size distribution. Mechanochemical and sonochemical effect of talc was determine via X-ray diffraction. Particle shape and surface texture of the ground and sonicated product was determined via scanning electron microscope and transmission electron microscope. The ground particle size exhibited particle size below 10 µm with narrow size distribution. The reduction of peak intensity in (002) plane indicated the layered structure has been distorted. The sonicated talc shows that the thickness of the talc particles after the sonication process is 20 nm but the lateral particle size still remains in micron range. The reduction of the XRD peak intensity for (002) plane and thickness of sonicated talc as shown in SEM and TEM micrographs proves that fine grinding and sonication process produces talc nanosheets.
Ultrasound technology progressed through the 1960’s from simple A-mode and B-mode scans to today’s M-mode and Doppler two dimensional (2-D) and even three dimensional (3-D) systems. Modern ultrasound imaging has its roots in sonar technology after it was first described by Lord John Rayleigh over 100 years ago on the interaction of acoustic waves with media. Tomography technique was developed as a diagnostic tool in the medical area since the early of 1970’s. This research initially focused on how to retrieve a cross sectional images from living or non-living things. After a decade, the application of tomography systems span into the industrial area. However, the long exposure time of medical radiation-based method cannot tolerate the dynamic changes in industrial process two phase liquid/gas flow system.. An alternative system such as a process tomography system, can give information on the nature of the flow regime characteristic. The overall aim of this paper is to investigate the use of a small scale ultrasonic tomography method based on ultrasonic transmission mode tomography for online monitoring of liquid/gas flow in pipe/vessel system through ultrasonic transceivers application. This non-invasive technique applied sixteen transceivers as the sensing elements to cover the pipe/vessel cross section. The paper also details the transceivers selection criteria, hardware setup, the electronic measurement circuit and also the image reconstruction algorithm applied. The system was found capable of visualizing the internal characteristics and provides the concentration profile for the corresponding liquid and gas phases.
The paper describes the uses of microfocus XRF to identify infected Basal Stem Rot (BSR) disease in Malaysian palm oil plants. Among symptoms of BSR are wilting of the leaves and plant malnutrition. The study involves determining the inorganic element content of normal and infected leaves. Si, Mo, Cl, K, Ca and Mn had been identified as the major elements. Their distribution was determined by constructing an elemental map of each of this element on the leaves. Line scan was also performed to look into changes on the element composition on a defined region. Quantitative analysis of Cl, Ca and K on the normal and infected leaves show that the infected leaves have lower Cl content and a higher Ca/K ratio than the normal leaves.
Currently, research in composite materials is being directed at using natural fibers instead of synthetics fibers. The use of natural fibers, derived from annually renewable resources, as reinforcing fibers in matrix provides positives environmental benefits with respect to ultimate disposability and raw material utilization. Natural fiber offers an alternative to the technical reinforcing fibers because of their low density, good mechanical performance, ultimate availability and disposability. Modifying the fiber surface by using chemical treatment can enhance bond strength between fiber and matrix. Chemical treatment also an effective way to clean the fiber surface, chemically modify the surface and increase the surface roughness. Surface analyses on fiber for before and after treatment were investigated using scanning electron microscopy (SEM).
The main purpose of this study was to analyzed and examined the cocoa butter samples from Sabah. This work presence the crystal phases present in cocoa butter sample thus proved the existence of polymorphs obtained from differential scanning calorimeter (DSC) analysis and confirmed by X-ray diffraction (XRD). The cocoa butter samples were extracted using a conventional method by Soxhlet Extraction method. Crystals were formed under controlled static and tempered conditions. Cocoa butter polymorphism demonstrates that it is the actual crystallization temperature, not the cooling rate that determines the polymorph that crystallizes.
The microstructural evolution of Sn-40Pb/Cu joints has been investigated under 125 o C thermal exposure conditions using single shear lap joints. A scanning electron microscope (SEM) was used to observe the morphology of the phases and energy dispersive x-ray (EDX) was used to estimate the elemental compositions of the phases. A double layer of Cu6Sn5 and Cu3Sn were observed. The Cu6Sn5 developed with a scalloped morphology, while the Cu3Sn always grew as a somewhat undulated planar layer in phase with the Cu6Sn5. The Cu6Sn5 layer began to transform from scallop shape to planar type after aging for 375 hours due to reduction in the interfacial energy. The intermetallic layers showed a linear dependence on the square root of aging time. The growth rate constant of the intermetallic compounds are estimated as 15.2 x 10 - 14 and 0.152 x 10 -14 cm 2 /s for Cu6Sn5 and Cu3Sn intermetallic, respectively.
The hardcoat anodising process was done by using different concentration of H2SO4 from 0% to 20%. The 90 volt of anodising process was applied by using Al foil as cathode materials. The surface changes on PM Al-Mg resulted by hardcoat anodising was characterised by XRD measured. Surface hardness was measured by Micro-Vickers hardness machine. The experiment found different XRD pattern between anodised PM Al-Mg samples. The study was found by that the optimum value for H2SO4 concentration was 15 % H2SO4 and result 26 μm thickness, 5.07% of mass changes and HVN 105.4 hardness. The hardcoat anodising was affected to the XRD pattern for PM Al-Mg.
Being an imperative material for man either used as building materials, pottery or as components in material industry and technology, knowledge of clays elemental contents is important. In the present study ten clay samples obtained from various locations in North-West Peninsular Malaysia were used. Majority of the clays were economically manufactured to be used as building materials or pottery. The objective of study was to determine the main elemental contents of the samples, and relate the results to the types of minerals, as well as to compare them with clays from other studies. In the study X-ray Fluorescence (XRF) coupled to samples dilution method and standard calibration samples was used. The elements detected in the study were Si, Al, Fe, Ti, K and Ca. Depending on locations, the percentage concentration ranged between 24.8 – 32.4 for Si, 10.8 – 19.0 for Al, 0.09 – 2.12 for Fe, 0.08 – 1.13 for Ti, 0.45 – 3.39 for K and trace amount of Ca and P. However, Mg that normally found in typical clay was not found in the studied samples. Comparing the oxide of the major elements with other studies, it was found that the clay samples contained mixtures of kaolinite (two-layered structure) and illite (three-layered structure).
α Cordierite is very important phase in MgO-Al2O3-SiO2 system because of their very outstanding thermal, chemical and electrical properties. In this presents study nonstoichiometry cordierite (MgO:Al2O3:SiO2 = 3:1.5:5) using 2 different initial raw materials ( (i)mixture of pure oxide, and ii) mainly mixture of minerals) were fabricated and compared in terms of phase transformation and physical properties. Cordierite was prepared by glass method at low melting temperature (1350°C). Low melting temperature has resulted in partly crystalline glass which has possesses higher hardness, required longer milling time and result in contamination from grinding media. However, α-cordierite has successfully crystallized and fully densified at 850°C/2h. Activation energy for densification was investigated from thermal expansion coefficient (TCE) results. Other properties that were discussed included thermal properties using DTA/TGA.
Phenolic resin-silica nanocomposites samples in pellet shape have been successfully prepared by intercalation of polymer solution through the hot pressing method. The phenolic resin is modified with organic elastomers of silica nanoparticles, which is about 20 nanometer in diameter. The change of density and porosity was studied based on the addition of silica content in the phenolic resin composites. The densities of composites increased with the addition of the silica content from 10 wt.% to 40 wt.%. On the other hand, the porosity percentage was decreased with increasing of silica contents. The mechanical properties (Young’s modulus, energy to break and time to failure) of the nanocomposites samples were identified using the Universal Testing Material Machine (UTM). The results of Young’s modulus, energy to break and time to failure of the phenolic resin composites were found to be slightly increased with silica content from 10 wt.% to 30 wt.%. The X-Ray Microtomogaphy (XRM) topographies have shown that the porosity exists on fracture structure for each nanocomposite. The nanocomposites surface structure has been analyzed using Scanning Electron Microscope (SEM). The observation shows that the fracture surface of the pure phenolic resin is relatively smooth and glassy, which is typical for a brittle material, but the phenolic resin- silica composites fracture surface is not smooth at all. The observations indicate the pure phenolic resin is brittle than phenolic resin-silica nanocomposites. Consequently, the physical properties of the phenolic resin-silica nanocomposites were improved with the addition of 10 wt.% to 30 wt.% silica contents, as compared to that of the pure phenolic resin.
In this paper, densification of in-situ copper-niobium carbide composite using cold pressing technique was addressed. Mixtures of Cu-20vol%NbC powder were prepared by two methods.
In first method, a mixture of Cu-15.79wt%Nb-2.04wt%C powder was milled at 400 rpm for 35 hours in a planetary mill. In second method, Cu and commercial NbC powder was mixed at 100 rpm for 2 hours in a jar mill. Then, both powders were pressed at different pressure (i.e. 350 MPa, 450 MPa, 550 MPa and 650 MPa) and sintered at 900 o C for 1 hour. Sample of in-situ and ex-situ Cu-20vol%NbC composite were characterized for density, hardness, phase formation by x-ray diffraction analysis and microstructure by scanning electron microscope. Xray diffraction analysis showed that NbC phase was formed in the in-situ processed sample. Hardness of in-situ processed copper composite was higher than that of the ex-situ processed copper composite due to good interface between coper matrix and niobium carbide reinforcement particle as well as distribution of finer niobium carbide particles in copper matrix. Sintered density of in-situ composite is lower than density of ex-situ composite beacuse of work hardening of the Cu-Nb-C mixture powder during powder to ball collision. Density and hardness of the in-situ and ex-situ Cu-20vol%NbC composites increase with the increase in compaction pressure as porosity is eliminated at higher compaction pressure.
In this study, natural Hydroxyapatite (HA) was extracted from clean cow bone by treatment with NaOH and heating at high temperature before ground into fine powder. The HA powder were than mixed together with binder for several hours. Dense HA were formed in die steel mould by using uniaxially pressing method. Sample was sintered at different temperature 1150, 1200, 1250 and 1300°C for several hours. The phases of specimen were identified using X-ray diffraction (XRD). The mechanical properties were analyzed using three-point bending testing and the microstructure was observed by scanning electron microscopy. From XRD results, natural HA shows phase of pure HA up to 1250 o C and fracture strength results indicated that the mechanical properties of specimen increase as temperature increase. From microstructure observation using SEM, HA specimen shows initial stages of sintering process at temperature 1150°C and show changes in microstructure evolution as temperature increase up to 1300°C.
Thin films of cerium oxide (CeO2) were prepared on silicon (Si) substrate by metal organic decomposition route. 0.25 M of cerium (III) acetylacetonate (acac) was used as starting materials with the addition of methanol and acetic acid as solvents. Oxide conversion of the film by thermal treatment was conducted at temperature ranging from 400 o C to 1000 o C for 15 min in argon ambient. X-ray diffraction (XRD) analysis utilizing Cukα radiation (Model Brukker’s Diffrac Plus ), Filmetrics system measurement, field emission scanning electron microscope (FE-SEM) (Model Zeiss Supra 35VP FE-SEM) and atomic force microscopy (AFM) (Model SII Nanonavi) were employed to characterize the phase formed and morphologies of the film produced.
Monodispersed and size-tunable nanocrystalline cobalt (Co) particles in the range of 100 to 400 nm are prepared by the reduction of Co(II) species in propylene glycol. Control of the particle size is achieved by varying the initial Co(II) species concentration and by the addition of nucleating agents. Smaller Co particles are produced with increasing amounts of Co(II) species and in the presence of nucleating agents. X-ray diffraction analysis (XRD) shows that the Co particles are predominantly face-centered cubic crystals of about 8-14 nm. The Co particles are also ferromagnetic at room temperature.
Ceramic materials play key role in several biomedical applications. One of them is bone graft which is use in treating bone defect which caused by injury or osteoporosis. Calcium phosphates based ceramic are preferred as bone grafts in hard tissue engineering because of their chemical compositions are similar to the composition of human bone, superior bioresorbable and bioactivity. In this study, β-tricalcium phosphate (β-TCP) ceramic was synthesized by using sol-gel method. Phosphorous pentoxide (P2O5) and calcium nitrate tetrahydrate (Ca(NO3)2.4H2O) were used as calcium and phosphate precursors. The effects of calcination temperature on the synthesis powder were studied using the XRD, SEM-EDS and FTIR techniques. It was found that calcination temperature greatly influence the purity of the synthesized powders. The β-TCP was the dominant phase with the formation of α-TCP at calcination temperature from 600 to 800°C. Pure β-TCP was obtained at calcination of 900°C. As the temperature increased to 1000°C, the β-TCP was decomposed to for calcium phosphate oxide (CPO). The sol-gel method has some advantages over other methods, mainly its simplicity and ability to produce pure β-TCP at lower calcination temperature.
Unaffected, affected and heavily affected teeth enamel were studied by using FT-Raman spectroscopy. The 14 permanent teeth’s enamel surface were measured randomly, resulting in total n=43 FT-Raman spectra. The results obtained from FT-Raman spectra of heavily affected, affected and unaffected tooth’s enamel surfaces did not show any significant difference. In this study, Kruskal-Wallis and Wilcoxon rank sum tests were used to compare the intensity between the categories of enamel as well as the surfaces of teeth samples.
One-dimensional nanostructure materials are very attractive because of their electronic and optical properties depending on their size. It is well known that properties of material can be tuned by reducing size to nanoscale because at the small sizes, that they behave differently with its bulk materials and the band gap will control by the size. The tunability of the band gap makes nanostructured materials useful for many applications. As one of the wide band gaps semiconductor compounds, zinc selenide (ZnSe) nanostructures (nanoparticles, nanowires, nanorods) have received much attention for the application in optoelectronic devices, such as blue laser diode, light emitting diodes, solar cells and IR optical windows. In this study, ZnSe nanostructures have been synthesized by reduction process of zinc selenate using hydrazine hydrate (N2H4.2H2O). The reductive agent of hydrazine hydrate was added to the starting materials of zinc selenate were heat treated at 500 o C for 1 hour under argon flow to form onedimensional nanostructures. The SEM and TEM images show the formation of nanocompositelike structures, which some small nanobars and nanopellets stick to the rod. The x-ray diffraction and elemental composition analysis confirm the formation of mixture zinc oxide and zinc selenide phases.
Phase composition of calcium phosphate ceramic is a characteristic directly related to the biological response of implants due to the differences in mechanical and biochemical properties of these compounds. The biodegradation rate of biphasic calcium phosphate (BCP) can be controlled by altering the HA to β-TCP ratios. In this study the crystalline phase evolution of BCP synthesized via precipitation from aqueous solution of (NH4)2PO4 titrated into heated solution of Ca (NO3)2 was evaluated. The resulting powder was fabricated into porous scaffold using polyurethane foam method. Bulk powders were sintered from 700 - 1400°C to determine the most significant sintering temperature to obtain a stable and well crystallize BCP phases. The porous scaffolds were then sintered at selected temperature and the effects of various sintering times from 5,7,9,11,13 and 15 h were investigated. Bulk powders were characterized by dilatometer, IR analysis and XRD and porous scaffolds were analyzed by XRD and SEMEdx. RIR method was performed to show that the HA to β-TCP ratios were increased with increasing of sintering time and reached the maximum HA value at 11h. It is found that, the possibilities to manipulate the HA to β-TCP ratios in BCP porous scaffold by just controlling the sintering time of the scaffold without controlling the starting powder characteristics.
Silicon nanostructures have successfully been synthesized by thermal evaporation technique using nickel catalyst. Silicon powder served as starting source material was evaporated at high temperature (900-1100°C) in inert carrier gas. The grown silicon nanostructures were collected on (111) silicon substrate surface that positioned at varied location from source material. By controlling heating rate, gas flow rate, growth temperature and time, substrate position and location; to the optimum condition produced the best quality at silicon nanostructures. In this work, the best parameter to produce silicon nanostructures is system ramping up 1000°C at 20°C/min heating rate, N2 flow at 100ml/min; silicon needle-like one dimensional silicon nanostructures growth on vertically-positioned substrate located at 12cm from source material for 1 hour growth time. The effects of these parameters on the structures and physical of nanostructures were characterized by field emission scanning electron microscope and x-ray diffraction.
In these studies, cordierite was mechanically synthesized after a sol-gel process. The effect of milling time of cordierite was investigated. Aluminium nitrate nonahydrate, magnesium nitrate hexahydrate and tetraethylorthosilicate (TEOS) were used as starting materials. Gels obtained were mechanically activated in planetary ball mill by at 300rpm grinding speed and grinding time (15min, 30min, 45min and 60min). Powders produced were characterized by X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscope (FESEM) and Energy Dispersive X-Ray (EDX). XRD analysis proved that α-cordierite was formed at lower temperature (1200°C) as compliment to without grinding, whereby it is formed at1300°C. FESEM analysis shows the size of the cordierite were in submicron scale. EDX analysis proved that magnesium, aluminium, silicon and oxygen are elements existed in cordierite.