Abstract: The purpose of this work was to synthesize and investigate phase formation, structure and thermophysical properties of the phosphates M0.5+xM'xZr2–x(PO4)3 (M – Cd, Sr, Pb; M' – Mg, Co, Mn). The compounds were synthesized by sol-gel method. The results showed formation of limited solid solutions of NZP/NASICON type. The crystal structures of triple phosphates of the compositions MMg0.5Zr1.5(PO4)3 were refined by the Rietveld method using XRD data. Heat capacity (8–660 K) of the phosphates Pb0.5+xMgxZr2-x(PO4)3 (x = 0, 0.5) was measured, and reversible polymorphic transitions were found at temperatures, close to the room temperature. The results of Rietveld structure refinement showed the polymorphism caused by disordering of lead cations in the cavities of NZP/NASICON structure. Thermal expansion (298−1073 K) of the phosphates MMg0.5Zr1.5(PO4)3 was studied by XRD method, and the compounds were found to belong to middle and low-expanding materials. Thermal diffusivity (298–573 K) of the ceramic samples of phosphates slightly decreased with temperature increasing. As was demonstrated, the studied phosphates are characterized by the better thermophysical characteristics than widespread fire-resistant materials, such as zirconia and etc.
Abstract: Zinc is a non-ferrous metal with potential application in orthopaedic implant materials. However, its poor mechanical properties were major challenge to its application. Therefore, this paper studies the mechanical properties of biodegradable Zn-based alloy for biomedical application. Pure zinc powder with varying (0, 1, 2, 3 & 6) wt% of magnesium powders were ball milled using ball-to-powder ratio (B:P) of 10:1 at 350 rpm for 4 hours. The resulting milled powders were compacted and sintered at 300 MPa and 350 °C respectively. Microstructural, phase and mechanical properties analyses were performed following American standard of testing and measurement. The results show that magnesium has influence on the mechanical properties of zinc. The compressive strength, hardness and elastic modulus of 210 ± 8.878 MPa, 76 ± 5.707 HV and 45 ± 11.616 GPa respectively as obtained in Zn-2Mg alloy were optimum and meet the minimum requirement of biodegradable metal for orthopaedics application. These results indicate an increase of 111, 93 and 93% in compressive strength, hardness and elastic modulus respectively as compared to pure zinc. The increase in mechanical properties was adduced to effectiveness of compaction pressure and intermetallic phase formation within the matrix resulting in high dislocation density for improving strength. The study concluded that, Zn-2Mg alloy with optimum mechanical properties can therefore be considered a potential candidate for orthopaedic application.
Abstract: Chemical doping with different elements and compounds at various amounts represents the most suitable approach to improve the superconducting properties of bismuth-based superconductors for technological applications. In this paper, the influence of partial substitution of Sr(BO2)2 for SrO on the phase formation kinetics and transport properties of (Bi,Pb)-2223 HTS has been studied for the first time. Samples with nominal composition Bi1.7Pb0.3Sr2-xCa2Cu3Oy[Sr(BO2)2]x, x=0, 0.0375, 0.075, 0.15, 0.25, were prepared by the standard solid state processing. The appropriate mixtures were calcined at 845 oC for 40 h. The resulting materials were pressed into pellets and annealed at 837 oC for 30 h in air. Superconducting properties of undoped (reference) and Sr(BO2)2-doped (Bi,Pb)-2223 compounds were investigated through X-ray diffraction (XRD), resistivity (ρ) and transport critical current density (Jc) measurements. The surface morphology changes in the prepared samples were examined by scanning electron microscope (SEM). XRD and Jc studies have shown that the low level Sr(BO2)2 doping (x=0.0375-0.075) to the Sr-site promotes the formation of high-Tc phase and leads to the enhancement of current carrying capacity in (Bi,Pb)-2223 HTS. The doped sample with x=0.0375 has the best performance compared to other prepared samples. The estimated volume fraction of (Bi,Pb)-2223 phase increases from ~25 % for reference specimen to ~70 % for x=0.0375. Moreover, strong increase in the self-field Jc value was observed for this dopant amount (Jc=340 A/cm2), compared to an undoped sample (Jc=110 A/cm2). Pronounced enhancement of superconducting properties of (Bi,Pb)-2223 superconductor can be attributed to the acceleration of high-Tc phase formation as well as the improvement of inter-grain connectivity by small amounts of Sr(BO2)2 dopant.
Abstract: Well-defined 2D Eu+3 co-doped ZrO2: Gd+3 nanoparticles were successfully synthesized by microwave assisted solution combustion technique for luminescent applications. The present investigation reports the rapid and effective method for the synthesis of the Eu+3 co-doped ZrO2:Gd+3 nanoparticles and study of the luminescence behavior of Eu+3 ion in ZrO2:Gd+3 nanostructures. The optical properties of the prepared nanostructures were investigated by using UV-visible spectroscopy and photoluminescence spectra. The phase formation and the morphology of the nanoplatelets were studied by XRD, FESEM and HRTEM. The average grain size was found to be 45-50 nm. The presence of Gd3+ ion increases the crystallinity of the material and hence acts as a good nucleating agent. The ZrO2:Gd3+ co-doped with Eu+3 nanoplatelets gives an emission at 607 nm, a strong red emission under the excitation wavelength of 255 nm.
Abstract: NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and
Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by
mechanochemical route in a planetary ball mill starting from mixture
of the appropriate quantities of the Ni(OH)2/Fe(OH)3,
Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide
powders. In order to monitor the progress of chemical reaction and
confirm phase formation, powder samples obtained after 25 h, 18 h
and 10 h of milling were characterized by X-ray diffraction (XRD),
transmission electron microscopy (TEM), IR, Raman and Mössbauer
spectroscopy. It is shown that the soft mechanochemical method, i.e.
mechanochemical activation of hydroxides, produces high quality
single phase ferrite samples in much more efficient way. From the IR
spectroscopy of single phase samples it is obvious that energy of
modes depends on the ratio of cations. It is obvious that all samples
have more than 5 Raman active modes predicted by group theory in
the normal spinel structure. Deconvolution of measured spectra
allows one to conclude that all complex bands in the spectra are made
of individual peaks with the intensities that vary from spectrum to
spectrum. The deconvolution of Raman spectra allows to separate
contributions of different cations to a particular type of vibration and
to estimate the degree of inversion.
Abstract: 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.
Abstract: 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.
Abstract: The powders of Ba(Ce1-xZrx)0.90Y0.1O3-δ (BCZY) with 0.2 ≤ x ≤ 0.6 have been prepared by a modified sol-gel method. Triethylenetetramine (TETA) was employed as chelating agent. Phase formation of calcined powders at 1100oC and sintered pellets at 1400oC of BCZY were examined by an X-ray diffractrometer (XRD). XRD results showed the calcined powder and sintered pellet formed a single perovskite phase over the entire range of x values. As the amount of zirconium substitution (x values) increase, the main peaks are shifted to the higher 2theta values which suggest a complete substitution of zirconium into cerium sites. All the obtained calcined powders and sintered pellets possess cubic structure (Pm-3m) at all x values.
Abstract: Metal matrix composites (MMCs) have gained a
considerable interest in the last three decades. Conventional powder
metallurgy production route often involves the addition of reinforcing
phases into the metal matrix directly, which leads to poor wetting
behavior between ceramic phase and metal matrix and the
segregation of reinforcements. The commonly used elements for
ceramic phase formation in iron based MMCs are Ti, Nb, Mo, W, V
and C, B. The aim of the present paper is to investigate the effect of
sintering temperature and V-B addition on densification, phase
development, microstructure, and hardness of Fe–V-B composites
(Fe-(5-10) wt. %B – 25 wt. %V alloys) prepared by powder
metallurgy process. Metal powder mixes were pressed uniaxial and
sintered at different temperatures (ranging from 1300 to 1400ºC) for
1h. The microstructure of the (V, B) Fe composites was studied with
the help of high magnification optical microscope and XRD.
Experimental results show that (V, B) Fe composites can be produced
by conventional powder metallurgy route.
Abstract: A theoretical approach to consider formation of chemical compound layer at the interface between initial substances A and B due to the interfacial interaction and diffusion is developed. It is considered situation when speed of interfacial interaction is large enough and diffusion of A-atoms through AB-layer is much more then diffusion of B-atoms. Atoms from A-layer diffuse toward B-atoms and form AB-atoms on the surface of B-layer. B-atoms are assumed to be immobile. The growth kinetics of the AB-layer is described by two differential equations with non-linear coupling, producing a good fit to the experimental data. It is shown that growth of the thickness of the AB-layer determines by dependence of chemical reaction rate on reactants concentration. In special case the thickness of the AB-layer can grow linearly or parabolically depending on that which of processes (interaction or the diffusion) controls the growth. The thickness of AB-layer as function of time is obtained. The moment of time (transition point) at which the linear growth are changed by parabolic is found.
Abstract: LTCC (Low Temperature Co-fired Ceramics) being the most advantageous technology towards the multilayer substrates for various applications, demands an extensive study of its raw materials. In the present work, a series of CuxMg1-xNb2O6 (x=0,0.4,0.6,1) has been prepared using sol-gel synthesis route and sintered at a temperature of 900°C to study its applicability for LTCC technology as the firing temperature is 900°C in this technology. The phase formation has been confirmed using X-ray Diffraction. Thermal properties like thermal conductivity and thermal expansion being very important aspect as the former defines the heat flow to avoid thermal instability in layers and the later provides the dimensional congruency of the dielectric material and the conductors, are studied here over high temperature up to the firing temperature. Although the values are quite satisfactory from substrate requirement point view, results have shown anomaly over temperature. The anomalous thermal behavior has been further analyzed using TG-DTA.
Abstract: In this study, the effect of mechanical activation on the synthesis of Fe3Al/Al2O3 nanocomposite has been investigated by using mechanochemical method. For this purpose, Aluminum powder and hematite as precursors, with stoichiometric ratio, have been utilized and other effective parameters in milling process were kept constant. Phase formation analysis, crystallite size measurement and lattice strain were studied by X-ray diffraction (XRD) by using Williamson-Hall method as well as microstructure and morphology were explored by Scanning electron microscopy (SEM). Also, Energy-dispersive X-ray spectroscopy (EDX) analysis was used in order to probe the particle distribution. The results showed that after 30-hour milling, the reaction was started, combustibly done and completed.
Abstract: Powder of La0.6Sr0.4CoO3-α (LSCO) was synthesized
by a combined citrate-EDTA method. The as-synthesized LSCO
powder was calcined, respectively at temperatures of 800, 900 and
1000 °C with different heating/cooling rates which are 2, 5, 10 and
15 °C min-1. The effects of heat treatments on the phase formation of
perovskite phase of LSCO were investigated by powder X-ray
diffraction (XRD). The XRD patterns revealed that the rate of
5 °C min-1 is the optimum heating/cooling rate to obtain a single
perovskite phase of LSCO with calcination temperature of 800 °C.
This result was confirmed by a thermogravimetric analysis (TGA) as
it showed a complete decomposition of intermediate compounds to
form oxide material was also observed at 800 °C.