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.
Electrodeposition of white copper-tin alloys (including white miralloys) has been done onto planar mild steel substrates from alkaline cyanide solutions at 65 0 C. The chemical composition of the coating is influenced by plating bath composition and current density. White miralloy can be produced from the test solution containing 10 g/l CuCN2 - , 45 g/l Na2SnO3, 25 g/l NaCN, and 12 g/l NaOH at current density about 5 mA/cm 2 . The local compositions of the coating cross section were analyzed using EDX installed in a FESEM operated at an accelerating voltage of 20 kV. The phases formed during co-deposition process were identified using XRD at 25 mA current and 35 kV voltage.
Indialite or α-cordierite was synthesized by glass crystallization method using mainly talc and kaolin and with small amount of MgO, Al2O3, SiO2 to compensate the chemical formulation of non-stoihiometric compositions of cordierite. (3MgO.1.5Al2O3.5SiO2). B2O3, P2O5 and CaO was also added to decrease the melting and sintering temperature of cordierite. The glasses were pelletized and sintered from 850 o C up to 1050 o C. Phase compositions of both heat treated glass was quantified by X-ray powder diffraction data by the Rietveld method using TOPAS Ver 3 software. Result shows that about 60wt% of α cordierite has successfully crystallized at 850 o C. Beside secondary phases (forsterite) which come from initial raw materials, phases from grinding media were also presents in the sample. The contamination was considered high since it has reacted with existence phases to form a new phase at higher temperature. Without any contamination from grinding it was expected to obtain more than 90wt% α cordierite using the same composition.
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.
Sodium silicate was used to synthesize silica fine particles at room temperature using non-ionic surfactant of triethanolamine (TEA), dissolution salt and precipitating agent. The experiments were conducted by different composition of precursor material, nonionic surfactant and dissolution salt concentrations through the sol-gel process. Various particle sizes in the range 100-300nm were synthesized. The particle size of silica powders were analyzed via Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-ray Analysis (EDAX), X-Ray Fluorescence (XRF), and Fourier Transformation Infrared (FTIR). The result has demonstrated that the particle size can be controlled by changing the ratio of non-ionic surfactant and dissolution salt or the sodium silicate concentration.
A study on the effect of the modify values of x in CaCu3-xMn4+xO12 system has been carried out with x = 0.1, 0.3, 0.5, 0.7 and 0.9. The materials were prepared via solid-state reaction. The preparation conditions have been optimized using thermogravimetry analysis (TGA) technique. Material formations under the reported conditions have been confirmed by X-ray diffraction (XRD) studies. The results show that the formation of CaCu3Mn4O12 started at calcinations temperature of 600 0 C with the presence of raw material and was formed completely at 850 0 C. Field emission scanning electron microscopy (FESEM) analysis indicated that the increase of x value in the composition had changed the microstructures to be more faceted. The impedance spectrum is characterized by the appearance of two semicircle arcs whose pattern of evolution changes with rise of values x in the CaCu3-xMn4+xMn4O12 system. Bulk resistance (Rb) and grain boundary resistance (Rgb) of CaCu3- xMn4+xO12 decreases form 824.24 : to 98.68 : and 418.18 : to 2.20 : respectively, with the increasing of x value.
The joining of ceramic-metal could be done through a few techniques: brazing, diffusion bonding, friction welding etc. However, the mechanism of ceramic-metal joining was still not properly understood. In this study, alumina rod was bonded to mild steel rod via friction welding technique by using Al 1100 sheet as interlayer. The diameter of the rods was 10 mm. Friction pressure of 20 MPa and forging pressure of 40 MPa were used. Rotational speeds were maintained at 900 rpm and friction times of 2 to 20 seconds were applied. The joining strength was determined through four point bending test. The maximum bending strength, 240 MPa was obtained at the friction times of 20 seconds. Under optical microscope and SEM observation, the deformation of the aluminum interface was clearly obtained. Mechanical interlocking and close contact between the aluminaaluminum and aluminum-mild steel were observed at magnifications of 3000X. The strength of alumina-steel bonding is much dependent on the wettability of the alumina surface by the molten aluminum and the existing of mechanical interlocking between interlayer and sample materials.
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.
CaCu3Ti4O12 was synthesized starting from a solution of TiO2 to which Ca and Cu nitrates were added. Due to the differences in the solubilities of the Ca, Cu and Ti, initial variations from ideal stoichiometry and a high solution pH was necessary to obtain stoichiometric CaCu3Ti4O12 precipitates. As precipitated samples were amorphous with CuO phases observed after drying of the precipitates at 300 oC. CaCu3Ti4O12 phases were observed after heat treatment at 1000 oC. XRD studies show the presence of CuO and TiO2 in addition to the CaCu3Ti4O12 for non stoichiometric samples. Observations under the SEM show the presence of Cu rich and Ti rich phases in addition to the CaCu3Ti4O12.
Ceramic foams are a class of high porosity materials that are used or being considered for a wide range of technological applications. Ceramic foam was produce by polymer replication method. In this process, commercial polymeric sponge was use as template, dipping with ceramic particles slurry, drying and then sintered to yield a replica of the original foams. The study was focus on the fabrication of different density of ceramic foams by varying the density of ceramic slurries (1.1876, 1.2687, 1.3653 and 1.5295 g/cm3). Properties of ceramic foam produced such as density was characterized accordingly to ASTM C 271-94 and porosity were characterized using Archimedes methods. Compressive and bending strength was performed accordingly to ASTM C1161-94 and C773-88 (1999), respectively. The morphological study was performed using Scanning Electron Microscopy (SEM) and EDX. Density of ceramic foams produced was about 0.5588 and 1.1852 g/cm3, where as porosity was around 26.28 and 70.59 %. Compressive and bending strength was increase from strength also increases from 2.60 to 23.07 MPa and 1.20 to 11.10 MPa, respectively, with increasing of slurries density from 1.1876 to 1.3653 g/cm3. The SEM micrographs show that the cells structure become denser as the slurries density increased. EDX proved that the ceramic used is porcelain. As a conclusion, increasing in slurries density produced ceramic foams with good mechanical properties such as compressive and bending strength and denser body.
Many attempts have been focused in the past on preparing of synthetic E-tricalcium (E-TCP), which being employed as bone substitute due to its biocompatibility and resorbability. Low temperature synthesize such as sol-gel method become popular due to the high product purity and homogenous composition. Sol-gel method is less economical towards commercialization because the cost of raw materials and the yield of the product that can be achieved. This paper describes the synthesis of ETCP via mixing of CaCO3 and H3PO4 followed by calcinations process at 750qC – 1050qC. X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimeter (DSC), fourier transformation infra-red (FTIR) were used for characterization and evaluation of the phase composition, morphology, particle size and thermal behavior of the product. E-TCP phase start to occur after calcinations at 750qC.
Ni–SiC composite coatings were electrodeposited from a Watts-type bath containing 5 g/l SiC particles in suspension. The particles were dispersed with the aid of mechanical agitation at 75 rpm and 150 rpm. EDX analysis confirmed the existence of Ni and SiC in the coatings. The effects of agitation speed on hardness properties of the coatings were investigated. SEM results showed that lower agitation speed could improve the amount of co-deposited SiC particles and increase the hardness of the composite coatings. The bonding between the Ni metal matrix and the SiC ceramic particles was compact.
Barium strontium titanate (Ba0.7Sr0.3TiO3) powder was processed at temperature 80 o C by reacting titania sol in aqueous solutions that contained BaCl2, SrCl2 and NaOH at atmospheric pressure.
The structural characteristic of the powder and sintered pellet were studied using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) whereas the electrical characteristic was determined via Impedance Spectroscopy (IS) and LCR meter. The synthesized powder was found to have a tetragonal phase after heating at 1300 o C. XRD pattern also showed the presence of secondary phase BaTi2O5 (BT2). The SEM results shows the fine grain size was in the range of 0.2 Pm to 0.4 Pm whereas the large ones are approximately 0.8 Pm to 1.2 Pm The ac response of sample sintered at 1300 o C indicated that three electrically different regions. Element 1 can be assigned as a ferroelectric grain boundary region and it is actually BT2, element 2 as a ferroelectric bulk region and the third element is a conductive core which has a low resistance (200 :) and capacitance value.
Dielectric material CaCu3Ti4O12 (CCTO) prepared by solid state technique, was calcined at different temperatures (700 - 1000 o C) for 6 and 12 hours. The calcined powder were analysed by XRD to identify the CCTO formation. Then the microstructure was observed by SEM. The CCTO single phase formation was firstly detected on sample calcined at 700 o C for 12 hours. The microstructure obtained shows the particles were spherical in shape. The grain getting larger as calcination temperature was increased.
A study of wear behaviour on anodised PM aluminium matrix composites (AMC) reinforced with Saffil™ alumina short fibres was done. AMC was fabricated by powder metallurgy methods (PM) with using Al flake powders and Saffil™ alumina short fibres. AMC reinforced with 15 wt % Saffil¥ alumina short fibre was selected because it showed optimum mechanical and physical properties. Sulphuric acid anodising process was performed and the objective is to obtain suitable parameters of sulphuric acid concentration, anodising voltage and anodising time on MMC. The study of anodising process was carried out with various sulphuric acid concentrations (from 0 to 20 % volume), anodising voltage (10 V to 20 V) and anodising time (from 0 to 60 minutes) at room temperature. Scanning electron microscope (SEM) was used to investigate coating morphology and thickness. From the research, anodising voltage of 18 V and 15 % vol H2SO4 in anodising time of 60 minutes were suitable parameters for sulphuric acid anodising of this AMC. SEM showed the coating thickness around 20 Pm. From the reserch, it was found that H2SO4 anodising was able to give good coating to MMC.
In this study the intermetallic (IMC) thickness of Sn-Pb, Sn-Zn and Sn-Zn-Bi solders on copper (Cu) substrate were measured at different temperatures using reflow methods. Cu6Sn5 intermetallic phase was detected between Sn-Pb solder and Cu substrate. The J-Cu5Zn8 phase was detected between Sn-Zn and Sn-Zn-Bi lead-free solders with Cu substrate. The thickness of the intermetallics increases with temperature. The IMC thickness for Sn-8Zn-3Bi solder is lower than Sn-9Zn solder for all the soldering temperatures, indicating that Bi has suppressed the initial IMC formation.
Triyttrium Pentairon (iii) Oxide (Y3Fe501,2) or familiar called as Yttrium Iron Garnet (YIG) is successfully prepared using a conventional mixed-oxide method of 5:3 Fe to Y ratios. YIG prepared from conventional mixed-oxide usually produced some associated phase which surely will affect electrical properties. In this study, various temperature used in the sintering process to induce associated phases (YIP) to be fully reacting to form single phase of YIG and the effect on resonance frequency is studied for resonator applications. The mixtures of oxide powders are calcined at 1100 "C and sintered at various temperatures of (1350, 1380, 1400, 1420 1450 QC, respectively). Cubic phase is detected from the formation of YIG. Some other phases such as YIP and hematite also present as secondary phase. However, it is seen that, based on the Rietvield refinement method, the total amount of secondary phase simulated are inversely proportional with sintering temperature. The powder was pressed into cylindrical pellet and tested as a microwave resonator in antenna application. It was found that, on the actual antenna circuit the operating frequencies measured are in the range of 10-12 GHz for all samples which suitable for X-band. At the end, overall radiation pattern for all samples exhibit an omnidirectional behavior.
The microstructure and mechanical properties of ceramic composites produced from alumina, yttria stabilized zirconia and chromia oxide system was investigated. The Cr2O3 weight percent was varied from 0 wt% to 1.0 wt%. Each batch of composition was mixed, uniaxially pressed to 13mm diameter and sintered at 1600 ◦C for 4 h in pressureless conditions. Studies on the effects of the sample microstructures on their mechanical and physical properties such as fracture toughness and bulk density were carried out. Results show that an addition of 0.6 wt% of Cr2O3 produces the best mechanical properties. Furthermore, microstructural observations show that the Al2O3 grain size is significantly dependent on the amount of Cr2O3 additives used. Maximum value obtained with 0.6 wt % Cr2O3 for the fracture toughness is 5.36 MPa.m1/2.
β-tricalcium phosphate (β-TCP) powders were synthesized by using various particles sizes (40 nm – 780 μm) calcium carbonate (CaCO3) and phosphoric acid (H3PO4) at room temperature (25 ˚C). The synthesized powders were characterized by using X-Ray Diffraction (XRD) method. The purity of β-TCP powders were determined from XRD pattern while the crystallite size of β-TCP powders were calculated by using Scherrer equation. Results shows that the purity of β-TCP powders were ranged from 20.33 % to 81.94 % while the crystallite size of β- TCP powders were ranged from 0.04391 μm to 0.06751 μm. From this work, particle size of CaCO3 will influenced the purity but not the mean crystallite size of synthesized β-TCP.
A co-deposition of nickel-phosphorus-alumina (NiPA) composite coatings were obtained from an ordinary sulphate-based plating bath consisting of 5 g/l alumina (Al2O3) particles. The particles were dispersed by using mechanical agitation at 125 rpm. The presence of Ni3P and Al2O3 phases in the coatings was confirmed by XRD analysis. SEM/EDX results indicated that a smooth Ni3P coating was obtained and Al2O3 particles were embedded into the coating. Microscopic observation showed that the bonding between the Ni3P metal matrix and the Al2O3 ceramic particles was compact.