• Issue front cover thumbnail

      Volume 30, Issue 4

      August 2007,   pages  301-426

    • Adhesive B-doped DLC films on biomedical alloys used for bone fixation

      A A Ahmad A M Alsaad

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      The long-term failure of the total hip and knee prostheses is attributed to the production of wear particles at the articulating interface between the metals, ceramics and polymers used for surgical implants and bone-fixtures. Therefore, finding an adhesive and inert coating material that has low frictional coefficient should dramatically reduce the production of wear particles and hence, prolong the life time of the surgical implants. The novel properties of the non-toxic diamond-like carbon (DLC) coatings have proven to be excellent candidates for biomedical applications. However, they have poor adhesion strength to the alloys and biomaterials. The addition of a thin interfacial layer such as Si, Ti, TiN, Mo and Cu/Cr and/or adding additives such as Si, F, N, O, W, V, Co, Mo, Ti or their combinations to the DLC films has been found to increase the adhesion strength substantially. In our study, grade 316L stainless steel and grade 5 titanium alloy (Ti–6Al–4V) were used as biomaterial substrates. They were coated with DLC films containing boron additives at various levels using various Si interfacial layer thicknesses. The best film adhesion was achieved at 8% and 20% on DLC coated Ti–6Al–4V and grade 316L substrates, respectively. It has been demonstrated that doping the DLC with boron increases their adhesion strength to both substrates even without silicon interfacial layer and increases it substantially with optimum silicon layer thickness. The adhesion strength is also correlated with the hydrogen contents in the B-DLC films. It is found to reach its maximum value of 700 kg/cm2 and 390 kg/cm2 at 2/7 and 3/6 for CH4/Ar partial pressures (in mTorr ratio) for Ti–6Al–4V and 316L substrates, respectively.

    • Characteristics of porous zirconia coated with hydroxyapatite as human bones

      V V Narulkar S Prakash K Chandra

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      Since hydroxyapatite has excellent biocompatibility and bone bonding ability, porous hydroxyapatite ceramics have been intensively studied. However, porous hydroxyapatite bodies are mechanically weak and brittle, which makes shaping and implantation difficult. One way to solve this problem is to introduce a strong porous network onto which hydroxyapatite coating is applied. In this study, porous zirconia and alumina-added zirconia ceramics were prepared by ceramic slurry infiltration of expanded polystyrene bead compacts, followed by firing at 1500°C. Then slurry of hydroxyapatite–borosilicate glass mixed powder was used to coat the porous ceramics, followed by firing at 1200°C. The porous structures without the coating had high porosities of 51–69%, high pore interconnectivity, and sufficiently large pore window sizes (300–500 𝜇m). The porous ceramics had compressive strengths of 5.3∼36.8 MPa, favourably comparable to the mechanical properties of cancellous bones. In addition, porous hydroxyapatite surface was formed on the top of the composite coating, whereas a borosilicate glass layer was found on the interface. Thus, porous zirconia-based ceramics were modified with a bioactive composite coating for biomedical applications.

    • Optical properties of CeO2 thin films

      S Debnath M R Islam M S R Khan

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      Cerium oxide (CeO2) thin films have been prepared by electron beam evaporation technique onto glass substrate at a pressure of about 6 × 10-6 Torr. The thickness of CeO2 films ranges from 140–180 nm. The optical properties of cerium oxide films are studied in the wavelength range of 200–850 nm. The film is highly transparent in the visible region. It is also observed that the film has low reflectance in the ultra-violet region. The optical band gap of the film is determined and is found to decrease with the increase of film thickness. The values of absorption coefficient, extinction coefficient, refractive index, dielectric constant, phase angle and loss angle have been calculated from the optical measurements. The X-ray diffraction of the film showed that the film is crystalline in nature. The crystallite size of CeO2 films have been evaluated and found to be small. The experimental 𝑑-values of the film agreed closely with the standard values.

    • Photoelectrochemical (PEC) studies on CdSe thin films electrodeposited from non-aqueous bath on different substrates

      Y G Gudage N G Deshpande A A Sagade R P Sharma S M Pawar C H Bhosale

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      Thin films of CdSe were deposited by potentiostatic mode on different substrates such as stainless steel, titanium and fluorine tin–oxide (FTO) coated glass using non-aqueous bath. The preparative parameters were optimized to get good quality CdSe thin films. These films were characterized by X-ray diffraction (XRD), optical absorption and photoelectrochemical (PEC) techniques. XRD study revealed that the films were polycrystalline in nature with hexagonal phase. Optical absorption study showed that CdSe films were of direct band gap type semiconductor with a band gap energy of 1.8 eV. PEC study revealed that CdSe film deposited on FTO coated glass exhibited maximum values of fill factor (FF) and efficiency (𝜂) as compared to the films deposited on stainless steel and titanium substrate.

    • Film adhesion in amorphous silicon solar cells

      A R M Yusoff M N Syahrul K Henkel

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      A major issue encountered during fabrication of triple junction 𝑎-Si solar cells on polyimide substrates is the adhesion of the solar cell thin films to the substrates. Here, we present our study of film adhesion in amorphous silicon solar cells made on different polyimide substrates (Kapton VN, Upilex-S and Gouldflex), and the effect of tie coats on film adhesion.

    • A re-look at critical factors influencing single-phase formation of Ba2Ti9O20 microwave dielectrics

      Unnikrishnan Gopinath Dhanya Chandran Seema Ansari Bindu Krishnan Rani Panicker Raghu Natarajan

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      The present study focuses on critical factors limiting single-phase formation of Ba2Ti9O20 (2 : 9). Apart from 2 : 9, other polytitanates that are richer in Ti or Ba could also be prepared as single-phase material without any stabilizing agent through chemical co-precipitation. 2 : 9 is found to be a stoichiometric compound and even 0.5% excess Ti or Ba leads to multiphase formation. Single-phase 2 : 9 could be achieved even through solid-state route without the addition of stabilizing agents using high purity raw materials. The present results do not agree with existing hypotheses viz. diffusion, high surface and nucleation energy, potential barrier, non-stoichiometry etc as critical factors limiting formation of 2 : 9 as single-phase material.

    • Thermal decomposition of natural dolomite

      S Gunasekaran G Anbalagan

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      Thermal decomposition behaviour of dolomite sample has been studied by thermogravimetric (TG) measurements. Differential thermal analysis (DTA) curve of dolomite shows two peaks at 777.8°C and 834°C. The two endothermic peaks observed in dolomite are essentially due to decarbonation of dolomite and calcite, respectively. The TG data of the decomposition steps have also been analysed using various differential, difference-differential and integral methods, viz. Freeman–Carroll, Horowitz–Metzger, Coats–Redfern methods. Values of activation entropy, Arrhenius factor, and order of reaction have been approximated and compared. Measured activation energies vary between 97 and 147 kJ mol-1. The large fluctuation in activation energy is attributed to the presence of impurities such as SiO2, Al2O3, Fe2O3, Cl- etc in the samples. FTIR and XRD analyses confirm the decomposition reaction. SEM observation of the heat-treated samples at 950°C shows cluster of grains, indicating the structural transformation.

    • Effect of nickel substitution on thermal properties of Na0.9CoO2

      J Meena Devi N Gayathri A Bharathi K Ramachandran

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      We report on the effect of nickel substitution in Na0.9CoO2 by examining their thermal properties at room temperature. Experimental results indicate that thermoelectric efficiency is enhanced upon nickel substitution in sodium cobaltate.

    • Growth and characterization of pure and lithium doped strontium tartrate tetrahydrate crystals by solution–gel technique

      B Suresh Kumar M H Rahim Kutty M R Sudarsana Kumar K Rajendra Babu

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      The effect of lithium ion as dopant on the size and transparency of strontium tartrate tetrahydrate (SrC4H4O6.4H2O) crystals are presented in this paper. Growth of single crystals of undoped and lithium doped strontium tartrate tetrahydrate by controlled diffusion of strontium nitrate into the gel charged with tartaric acid at room temperature are narrated. The lithium ion enhances the size and transparency of the doped crystals. The crystal structure of the compound was confirmed by X-ray diffractometry and dopant concentration with ICP–atomic emission spectrometer system. Thermal decomposition of the grown crystals is investigated by TGA and DTA studies. The FTIR spectra of pure and doped crystals are recorded and analysed. Kurtz powder technique has been used to test SHG efficiency of the crystals.

    • Dielectric, elastic, anelastic and conductivity behaviour of ferroelectromagnetic composites, Ni0.5Zn0.5Fe1.95O4–𝛿 + Ba0.8Pb0.2TiO3

      N Ramamanohar Reddy M Venkata Ramana K Krishnaveni K V Siva Kumar V R K Murthy

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      Ferroelectromagnetic composites with compositions, 𝑋 Ni0.5Zn0.5Fe1.95O4–𝛿 + (1 – 𝑋) Ba0.8Pb0.2TiO3, in which 𝑋 varies as 0, 0.005, 0.010, 0.015, 0.020, 0.040, 0.060, 0.080 and 1 in mole %, were prepared by conventional ceramic double sintering process. The presence of two phases was confirmed by X-ray diffraction. The temperature variation of dielectric constant, 𝜀', dielectric loss, tan 𝛿, d.c. conductivity, a.c. conductivity, elastic and anelastic behaviour of ferrite–ferroelectric composites were studied in the temperature range 30–350°C. The a.c. conductivity measurements on these composites in the frequency range 100 Hz–1 MHz at room temperature reveal that the conduction mechanism is due to small polaron hopping. The dielectric and elastic data were discussed in the light of phase transitions.

    • Macrovoids formation and light scattering of PMMA

      Zhi Hong Chen Z C Chang C B Lin

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      After desorption of PMMA with saturated methanol and ethanol and then desorption by distilled water, the macrovoids are formed because of the phase inversion. The macrovoids on the surface of the specimens are larger and more numerous than those in the bulk. The macrovoids are likely to be closed-type, if the hydrolysis temperature is lower. On the other hand, if the hydrolysis temperature is higher, the macrovoids are likely to be open-type. Due to the formation of macrovoids, smaller than visible wavelengths, the light will disperse, and therefore, reduces the transmittance of the specimens. The transmittance is decreased when the hydrolysis temperature and hydrolysis time are increased. Furthermore, it is much clearer when ethanol is used as solvent than methanol. The scattered intensity of the specimens after hydrolysis is inversely proportional to the visible wavelength with an exponent, 𝑛, in the range 0.04–2.83 for methanol and 0.02–0.21 for ethanol.

    • Carbon nanotube reinforced polymer composites—A state of the art

      S Bal S S Samal

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      Because of their high mechanical strength, carbon nanotubes (CNTs) are being considered as nanoscale fibres to enhance the performance of polymer composite materials. Novel CNT-based composites have been fabricated using different methods, expecting that the resulting composites would possess enhanced or completely new set of physical properties due to the addition of CNTs. However, the physics of interactions between CNT and its surrounding matrix material in such nano-composites has yet to be elucidated and methods for determining the parameters controlling interfacial characteristics such as interfacial shear stress, is still challenging. An improvement of the physical properties of polymer nanocomposites, based on carbon nanotubes (CNTs), is addicted to a good dispersion and strong interactions between the matrix and the filler.

    • Selective absorption of water from different oil–water emulsions with Psy-cl-poly(AAm) synthesized using irradiation copolymerization method

      B S Kaith Kiran Kumar

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      The present paper deals with the functionalization of psyllium with acrylamide under the influence of gamma radiation using hexamethylene tetramine as a crosslinker. The polymer synthesized was characterized using FTIR spectroscopy, scanning electron microscopy and thermogravimetric analysis. The superabsorbent was then used further for the selective absorption of water from different oil–water emulsions.

    • Separation of matrix alloy and reinforcement from aluminum metal matrix composites scrap by salt flux addition

      K R Ravi R M Pillai B C Pai M Chakraborty

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      Separation of matrix alloy and reinforcements from pure Al–SiCp composite scrap by salt flux addition has been theoretically predicted using interface free energies. Experiments performed confirm the theoretical prediction. Complete separation of matrix aluminum and reinforcement from metal matrix composites (MMCs) scrap has been achieved by addition of 2.05 wt% of equimolar mixture of NaCl–KCl salt flux with a metal and particle yield of 84 and 50%, respectively. By adding 5 wt% of NaF to equimolar mixture of NaCl–KCl, metal and particle yield improved to 91 and 73%, respectively. Reusability of both the matrix aluminum and the SiC separated from Al–SiCp scraps has been analysed using XRD, SEM and DTA techniques. The matrix alloy separated from Al–SiCp scraps can be used possibly as a low Si content Al–Si alloy. However, the interfacial reaction that occurred during the fabrication of the composites had degraded the SiC particles.

    • Ceramic coated Y1 magnesium alloy surfaces by microarc oxidation process for marine applications

      V V Narulkar S Prakash K Chandra

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      The magnesium alloys occupy an important place in marine applications, but their poor corrosion resistance, wear resistance, hardness and so on, have limited their application. To meet these defects, some techniques are developed. Microarc oxidation is a one such recently developed surface treatment technology under anodic oxidation in which ceramic coating is directly formed on the surface of magnesium alloy, by which its surface property is greatly improved. In this paper, a dense ceramic oxide coating, ∼ 20 𝜇m thick, was prepared on an Y1 magnesium alloy through microarc oxidation in a Na3SiO3–Na2WO4–KOH–Na2EDTA electrolytic solution. The property of corrosion resistance of ceramic coating was studied by CS300P electrochemistry–corrosion workstation, and the main impact factor of the corrosion resistance was also analysed. Microstructure and phase composition were analysed by SEM and XRD. The microhardness of the coating was also measured. The basic mechanism of microarc coating formation is explained in brief.

      The results show that the corrosion resistance property of microarc oxidation coating on the Y1 magnesium surface is superior to the original samples in the 3.5 wt% NaCl solutions. The microarc oxidation coating is relatively dense and uniform, mainly composed of MgO, MgAl2O4 and MgSiO3. The microhardness of the Y1 magnesium alloy surface attained 410 HV, which was much larger than that of the original Y1 magnesium alloy without microarc oxidation.

    • Modelling of soft impingement during solidification

      K T Kashyap S Yamdagni

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      It has been well established that spheroidal grain morphology in the microstructure forms during stir casting (rheocasting) and grain refinement of magnesium alloys by zirconium addition. This curious microstructure has been of interest both commercially from enhanced mechanical properties and also scientific interest in explaining the mechanism of spheroidal grain formation. Vogel and Doherty proposed a model describing the fracturing of dendrite arms during stir casting to produce a high density of nuclei which they presume to give rise to spheroidal grains. They proposed that there is soft impingement of diffusion fields of neighbouring nuclei, which reduces the concentration gradient ahead of the planar solid and liquid interface, which in turn negates shape instability. In this paper, the Vogel and Doherty model is pursued by quantitative modeling of soft impingement problem and related to shape instability by constitutional supercooling theory. This analysis correctly predicts the spheroidal grain formation during stir casting or rheocasting. This model can also be used to explain the grain refinement of magnesium alloys by zirconium addition wherein spheroidal grains are formed.

    • Structural phase transitions and piezoelectric anomalies in ordered Sc0.5Ga0.5N alloys

      A M Alsaad A A Ahmad

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      Local-density approximation calculations (LDA) within density functional theory (DFT) and Berry phase approach within modern theory of polarization are performed to predict the structural and piezoelectric properties of ordered Sc0.5Ga0.5N alloys under compressive and tensile in-plane strain. This alloy is found to exhibit a tremendous piezoelectric response, associated with a phase transition from nonpolar 𝑝63/𝑚𝑐𝑐(𝐷6h) space group to a polar 𝑝63𝑚𝑐(𝐶6v) structure, at fixed Ga and Sc compositions when continuously changing the experimental accessible parameters (i.e. the compressive and tensile strain). The mechanism of the effects behind such anomalous behaviour is revealed and explained.

    • Interfacial microstructure and strength of diffusion brazed joint between Al2O3–TiC and 9Cr1MoV steel

      Wang Juan Li Yajiang S A Gerasimov

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      Joining of composite, Al2O3–TiC, with heat-resistant 9Cr1MoV steel, was carried out by diffusion brazing technology, using a combination of Ti, Cu and Ti as multi-interlayer. The interfacial strength was measured by shear testing and the result was explained by the fracture morphology. Microstructural characterization of the Al2O3–TiC/9Cr1MoV joint was investigated by X-ray diffraction (XRD) and scanning electron microscope (SEM) with energy-dispersion spectroscopy (EDS). The results indicate that a Al2O3–TiC/9Cr1MoV joint with a shear strength of 122 MPa can be obtained by controlling heating temperature at 1130°C for 60 min with a pressure of 12 MPa. Multi-interlayer Ti/Cu/Ti was fused fully and diffusion occurred to produce interfacial layer between Al2O3–TiC and 9Cr1MoV steel. The total thickness of the interfacial layer is about 100 𝜇m and Ti3AlC2, TiC, Cu and Fe2Ti are found to occur in the interface layer.

    • XRD and FT–IR investigations of sub-bituminous Assam coals

      Binoy K Saikia R K Boruah P K Gogoi

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      Two coal samples collected from Makum coal field, Assam, India were studied by XRD and FT–IR techniques. The X-ray diffractogram shows the existence of some crystalline carbons in Assam coals as proven by the appearance of peaks. The radial distribution functional (RDF) method was applied for the determination of structural aspects of the coals. The study indicates that the coals are lignite in type and there is no evidence of graphite-like structures. The maximum in the 𝐺(𝑟) plots of function of radial distribution of atoms (FRDA) relates to different distances between carbon atoms of aliphatic chains. The first significant maximum relates to the C–C bond (type C–CH=CH–C), the second maximum relates to the distance between carbon atoms of aliphatic chains that are located across one carbon atom. The curve intensity profiles obtained from FRDA show quite regular molecular packets for this coal. The coals were found to be lignite in nature. FT–IR study shows the presence of aliphatic carbon, C=O and C–O stretching associated with –OH and –NH stretching vibrations. Kaolinite and quartz were also found to be major minerals in Assam coals by FTIR spectroscopy. The difference in intensities of carbonyl groups of the coal samples is likely to relate with the rank.

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