Abstract: NiTi alloys possess magnificent superelastic, shape memory, high strength and biocompatible properties. For improving mechanical properties, foremost, superelasticity behavior, heat treatment process is carried out. In this paper, two different heat treatment methods were undertaken: (1) solid solution, and (2) aging. The effect of each treatment in a constant time is investigated. Five samples were prepared to study the structure and optimize mechanical properties under different time and temperature. For measuring the upper plateau stress, lower plateau stress and residual strain, tensile test is carried out. The samples were aged at two different temperatures to see difference between aging temperatures. The sample aged at 500 °C has a bigger crystallite size and lower amount of Ni which causes the mentioned sample to possess poor pseudo elasticity behaviour than the other aged sample. The sample aged at 460 °C has shown remarkable superelastic properties. The mentioned sample’s higher plateau is 580 MPa with the lowest residual strain (0.17%) while other samples have possessed higher residual strains. X-ray diffraction was used to investigate the produced phases.
Abstract: Manganese oxide is being recently used as electrode material for rechargeable batteries. In this study, Al incorporated Mn2O3 compositions were synthesized to study the effect of Al doping on electrochemical performance of host material. Structural studies were carried out using X-ray diffraction analysis to confirm the phase stability and explore the lattice parameters, crystallite size, lattice strain, density and cell volume. Morphology and composition were analyzed using field emission scanning electron microscope and energy dispersive X-ray spectroscopy, respectively. Dynamic light scattering analysis was performed to observe the average particle size of the compositions. FTIR measurements exhibit the O-Al-O and O-Mn-O and Al-O bonding and with increasing the concentration of Al, the vibrational peaks of Mn-O become sharper. An enhanced electrochemical performance was observed in compositions with higher Al content.
Abstract: Lithium iron phosphate (LiFePO4) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO4 (LFP) and carbon-coated nanograined LiFePO4 (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg-1 as compared to non-coated and micrograined sized commercial LFP.
Abstract: A systematic study was conducted to explore the photocatalytic reduction of carbon dioxide (CO2) into methanol on TiO2 loaded copper ferrite (CuFe2O4) photocatalyst under visible light irradiation. The phases and crystallite size of the photocatalysts were characterized by X-ray diffraction (XRD) and it indicates CuFe2O4 as tetragonal phase incorporation with anatase TiO2 in CuFe2O4/TiO2 hetero-structure. The XRD results confirmed the formation of spinel type tetragonal CuFe2O4 phases along with predominantly anatase phase of TiO2 in the CuFe2O4/TiO2 hetero-structure. UV-Vis absorption spectrum suggested the formation of the hetero-junction with relatively lower band gap than that of TiO2. Photoluminescence (PL) technique was used to study the electron–hole (e−/h+) recombination process. PL spectra analysis confirmed the slow-down of the recombination of electron–hole (e−/h+) pairs in the CuFe2O4/TiO2 hetero-structure. The photocatalytic performance of CuFe2O4/TiO2 was evaluated based on the methanol yield with varying amount of TiO2 over CuFe2O4 (0.5:1, 1:1, and 2:1) and changing light intensity. The mechanism of the photocatalysis was proposed based on the fact that the predominant species of CO2 in aqueous phase were dissolved CO2 and HCO3- at pH ~5.9. It was evident that the CuFe2O4 could harvest the electrons under visible light irradiation, which could further be injected to the conduction band of TiO2 to increase the life time of the electron and facilitating the reactions of CO2 to methanol. The developed catalyst showed good recycle ability up to four cycles where the loss of activity was ~25%. Methanol was observed as the main product over CuFe2O4, but loading with TiO2 remarkably increased the methanol yield. Methanol yield over CuFe2O4/TiO2 was found to be about three times higher (651 μmol/gcat L) than that of CuFe2O4 photocatalyst. This occurs because the energy of the band excited electrons lies above the redox potentials of the reaction products CO2/CH3OH.
Abstract: This work studies the effect of thickness on structural
and electrical properties of CuAlS2 thin films grown by two stage
vacuum thermal evaporation technique. CuAlS2 thin films of
thicknesses 50nm, 100nm and 200nm were deposited on suitably
cleaned corning 7059 glass substrate at room temperature (RT). In
the first stage Cu-Al precursors were grown at room temperature by
thermal evaporation and in the second stage Cu-Al precursors were
converted to CuAlS2 thin films by sulfurisation under sulfur
atmosphere at the temperature of 673K. The structural properties of
the films were examined by X-ray diffraction (XRD) technique while
electrical properties of the specimens were studied using four point
probe method. The XRD studies revealed that the films are of
crystalline in nature having tetragonal structure. The variations of the
micro-structural parameters, such as crystallite size (D), dislocation
density ( ), and micro-strain ( ), with film thickness were
investigated. The results showed that the crystallite sizes increase as
the thickness of the film increases. The dislocation density and
micro-strain decreases as the thickness increases. The resistivity ( )
of CuAlS2 film is found to decrease with increase in film thickness,
which is related to the increase of carrier concentration with film
thickness. Thus thicker films exhibit the lowest resistivity and high
carrier concentration, implying these are the most conductive films.
Low electrical resistivity and high carrier concentration are widely
used as the essential components in various optoelectronic devices
such as light-emitting diode and photovoltaic cells.
Abstract: In this study, the effects and interactions of reaction
time and capping agent assistance during sol-gel synthesis of
magnesium substituted hydroxyapatite nanopowder (MgHA) on
hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P
ratio and mean crystallite size was examined experimentally as well
as through statistical analysis. MgHA nanopowders were synthesized
by sol-gel technique at room temperature using aqueous solution of
calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and
potassium dihydrogen phosphate as starting materials. The reaction
time for sol-gel synthesis was varied between 15 to 60 minutes. Two
process routes were followed with and without addition of
triethanolamine (TEA) in the solutions. The elemental compositions
of as-synthesized powders were determined using X-ray fluorescence
(XRF) spectroscopy. The functional groups present in the assynthesized
MgHA nanopowders were established through Fourier
Transform Infrared Spectroscopy (FTIR). The amounts of phases
present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders
were determined using X-ray diffraction (XRD). The HA content in
biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized
MgHA nanopowders increased effectively with reaction time of sols
(p0.15, two way ANOVA). The MgHA nanopowders
synthesized with TEA assistance exhibited 14 nm lower crystallite
size (p
Abstract: Pure nickel coatings have been successfully
electrodeposited on copper substrates by the pulse plating technique.
The influence of current density, duty cycle and pulse frequency on
the surface morphology, crystal orientation, and microhardness was
determined. It was found that the crystallite size of the deposit
increases with increasing current density and duty cycle. The crystal
orientation progressively changed from a random texture at 1 A/dm2
to (200) texture at 10 A/dm2. Increasing pulse frequency resulted in
increased texture coefficient and peak intensity of (111) reflection.
An increase in duty cycle resulted in considerable increase in texture
coefficient and peak intensity of (311) reflection. Coatings obtained
at high current densities and duty cycle present a mixed morphology
of small and large grains. Maximum microhardness of 193 Hv was
achieved at 4 A/dm2, 10 Hz and duty cycle of 50%. Nickel coatings
with (200) texture are ductile while (111) texture improves the
microhardness of the coatings.
Abstract: The aim of this study was to investigate the
photocatalytic activity of polycrystalline phases of bismuth tungstate
of formula Bi2WO6. Polycrystalline samples were elaborated using a
coprecipitation technique followed by a calcination process at
different temperatures (300, 400, 600 and 900°C). The obtained
polycrystalline phases have been characterized by X-ray diffraction
(XRD), scanning electron microscopy (SEM), and transmission
electron microscopy (TEM). Crystal cell parameters and cell volume
depend on elaboration temperature. High-resolution electron
microscopy images and image simulations, associated with X-ray
diffraction data, allowed confirming the lattices and space groups
Pca21. The photocatalytic activity of the as-prepared samples was
studied by irradiating aqueous solutions of Rhodamine B, associated
with Bi2WO6 additives having variable crystallite sizes. The
photocatalytic activity of such bismuth tungstates increased as the
crystallite sizes decreased. The high specific area of the
photocatalytic particles obtained at 300°C seems to condition the
degradation kinetics of RhB.
Abstract: These Monolayer and multilayer coatings of CrN and
AlCrN deposited on 100Cr6 (AISI 52100) substrate by PVD
magnetron sputtering system. The microstructures of the coatings
were characterized using atomic force microscopy (AFM). The AFM
analysis revealed the presence of domes and craters that are
uniformly distributed over all surfaces of the various layers.
Nanoindentation measurement of CrN coating showed maximum
hardness (H) and modulus (E) of 14 GPa and 190 GPa, respectively.
The measured H and E values of AlCrN coatings were found to be 30
GPa and 382 GPa, respectively. The improved hardness in both the
coatings was attributed mainly to a reduction in crystallite size and
decrease in surface roughness. The incorporation of Al into the CrN
coatings has improved both hardness and Young’s modulus.
Abstract: Chitosan functionalized Fe3O4-Au core shell
nanoparticles have been prepared using a two-step wet chemical
approach using NaBH4 as reducing agent for formation of Au in
ethylene glycol. X-ray diffraction studies shows individual phases of
Fe3O4 and Au in the as prepared samples with crystallite size of 5.9
and 11.4 nm respectively. The functionalization of the core-shell
nanostructure with Chitosan has been confirmed using Fourier
transform infrared spectroscopy along with signatures of octahedral
and tetrahedral sites of Fe3O4 below 600cm-1. Mössbauer
spectroscopy shows decrease in particle-particle interaction in
presence of Au shell (72% sextet) than pure oleic coated Fe3O4
nanoparticles (88% sextet) at room temperature. At 80K, oleic acid
coated Fe3O4 shows only sextets whereas the Chitosan functionalized
Fe3O4 and Chitosan functionalized Fe3O4@Au core shell show
presence of 5 and 11% doublet, respectively.
Abstract: The objective of this work is to study the effect of two
key factors - external magnetic field and applied current density
during template-based electrodeposition of nickel nanowires using an
electrode distance of 20 mm. Morphology, length, crystallite size and
crystallographic characterization of the grown nickel nanowires at an
electrode distance of 20mm are presented. For this electrode distance
of 20 mm, these two key electrodeposition factors when coupled was
found to reduce crystallite size with a higher growth length and
preferred orientation of Ni crystals. These observed changes can be
inferred to be due to coupled interaction forces induced by the
intensity of applied electric field (current density) and external
magnetic field known as magnetohydrodynamic (MHD) effect during
the electrodeposition process.
Abstract: Violet Sr–Al–O:Eu2+ phosphor particles were
synthesized from a metal–ethylenediaminetetraacetic acid (EDTA)
solution of Sr, Al, Eu, and particulate alumina via spray drying and
sintering in a reducing atmosphere. The crystal structures and emission
properties at 85–300 K were investigated. The composition of the
violet Sr–Al–O:Eu2+ phosphor particles was determined from various
Sr–Al–O:Eu2+ phosphors by their emission properties’ dependence
on temperature. The highly crystalline SrAl12O19:Eu2+ emission phases
were confirmed by their crystallite sizes and the activation energies for
the 4f5d–8S7/2 transition of the Eu2+ ion. These results showed that the
material identification for the violet Sr–Al–O:Eu2+ phosphor was
accomplished by the low-temperature luminescence measurements.
Abstract: This article presents summary on preparation and
characterization of zinc, copper, cadmium and cobalt chromite
nanocrystals, embedded in an amorphous silica matrix. The
ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2
nanocomposites were prepared by a conventional sol-gel method
under acid catalysis. Final heat treatment of the samples was carried
out at temperatures in the range of 900−1200 ◦C to adjust the
phase composition and the crystallite size, respectively. The resulting
samples were characterized by Powder X-ray diffraction (PXRD),
High Resolution Transmission Electron Microscopy (HRTEM),
Raman/FTIR spectroscopy and magnetic measurements. Formation
of the spinel phase was confirmed in all samples. The average size of
the nanocrystals was determined from the PXRD data and by direct
particle size observation on HRTEM; both results were correlated.
The mean particle size (reviewed by HRTEM) was in the range from
∼4 to 46 nm. The results showed that the sol-gel method can be
effectively used for preparation of the spinel chromite nanoparticles
embedded in the silica matrix and the particle size is driven by the
type of the cation A2+ in the spinel structure and the temperature
of the final heat treatment. Magnetic properties of the nanocrystals
were found to be just moderately modified in comparison to the bulk
phases.
Abstract: In this paper, strontium ferrite (SrO.6Fe2O3) was
synthesized by the sol-gel auto-combustion process. The thermal
behavior of powder obtained from self-propagating combustion of
initial gel was evaluated by simultaneous differential thermal analysis
(DTA) and thermo gravimetric (TG), from room temperature to
1200°C. The as-burnt powder was calcined at various temperatures
from 700-900°C to achieve the single-phase Sr-ferrite. Phase
composition, morphology and magnetic properties were investigated
using X-ray diffraction (XRD), transmission electron microscopy
(TEM) and vibrating sample magnetometry (VSM) techniques.
Results showed that the single-phase and nano-sized hexagonal
strontium ferrite particles were formed at calcination temperature of
800°C with crystallite size of 27 nm and coercivity of 6238 Oe.
Abstract: In this research, n-dodecylthiol was added to P3HT/ PC70BM polymer solar cells to improve the crystallinity of P3HT and enhance the phase separation of P3HT/PC70BM. The improved crystallinity of P3HT:PC70BM doped with 0-5% by volume of n-dodecylthiol resulted in improving the power conversion efficiency of polymer solar cells by 33%. In addition, thermal annealing of the P3HT/PC70MB/n-dodecylthiolcompound showed further improvement in crystallinity with n-dodecylthiol concentration up to 2%. The highest power conversion efficiency of 3.21% was achieved with polymer crystallites size L of 11.2nm, after annealing at 150°C for 30 minutes under a vacuum atmosphere. The smaller crystallite size suggests a shorter path of the charge carriers between P3HT backbones, which could be beneficial to getting a higher short circuit current in the devices made with the additive.
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: Noble metal participation in nanostructured
semiconductor catalysts has drawn much interest because of their
improved properties. Recently, it has been discussed by many
researchers that Ag participation in TiO2, CuO, ZnO semiconductors
showed improved photocatalytic and optical properties. In this
research, Ag/ZnO nanocomposite particles were prepared by
Ultrasonic Spray Pyrolysis(USP) Method. 0.1M silver and zinc
nitrate aqueous solutions were used as precursor solutions. The
Ag:Zn atomic ratio of the solution was selected 1:1. Experiments
were taken place under constant air flow of 400 mL/min at 800°C
furnace temperature. Particles were characterized by X-Ray
Diffraction (XRD), Scanning Electron Microscope (SEM) and
Energy Dispersive Spectroscopy (EDS). The crystallite sizes of Ag
and ZnO in composite particles are 24.6 nm, 19.7 nm respectively.
Although, spherical nanocomposite particles are in a range of 300-
800 nm, these particles are formed by the aggregation of primary
particles which are in a range of 20-60 nm.
Abstract: Platinum oxide nanoparticles were prepared by a
simple hydrothermal route and chemical reduction using
carbohydrates (Fructose and sucrose) as the reducing and
stabilizing agents. The crystallite size of these nanoparticles was
evaluated from X-ray diffraction (XRD), atomic force microscopy
(AFM) and transmission electron microscopy (TEM) and was
found to be 10 nm as shown in figure 1, which is the
demonstration of EM bright field and transmission electron
microscopy. The effect of carbohydrates on the morphology of the
nanoparticles was studied using TEM (Figure 1). The
nanoparticles (100 μg/ml) were administered to the Pseudomonas
Stutzeri and Lactobacillus cultures and the incubation was done at
35 oC for 24 hours. The nanocomposites exhibited interesting
inhibitory as well as bactericidal activity against P. Stutzeri and
and Lactobacillus species. Incorporation of nanoparticles also
increased the thermal stability of the carbohydrates.
Abstract: The effect of calcination temperature and MgO crystallite sizes on the structure and catalytic performance of TiO2 supported nano-MgO catalyst for the trans-esterification of soybean oil has been studied. The catalyst has been prepared by deposition precipitation method, characterised by XRD and FTIR and tested in an autoclave at 225oC. The soybean oil conversion after 15 minutes of the trans-esterification reaction increased when the calcination temperature was increased from 500 to 600oC and decreased with further increase in calcination temperature. Some glycerolysis activity was also detected on catalysts calcined at 600 and 700oC after 45 minutes of reaction. The trans-esterification reaction rate increased with the decrease in MgO crystallite size for the first 30 min.
Abstract: In this paper, Zinc Oxide (ZnO) thin films are deposited on glass substrate by sol-gel method. The ZnO thin films with well defined orientation were acquired by spin coating of zinc acetate dehydrate monoethanolamine (MEA), de-ionized water and isopropanol alcohol. These films were pre-heated at 275°C for 10 min and then annealed at 350°C, 450°C and 550°C for 80 min. The effect of annealing temperature and different thickness on structure and surface morphology of the thin films were verified by Atomic Force Microscopy (AFM). It was found that there was a significant effect of annealing temperature on the structural parameters of the films such as roughness exponent, fractal dimension and interface width. Thin films also were characterizied by X-ray Diffractometery (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure and show the c-axis grain orientation. Increasing annealing temperature increased the crystallite size and the c-axis orientation of the film after 450°C. Also In this study, ZnO thin films in different thickness have been prepared by sol-gel method on the glass substrate at room temperature. The thicknesses of films are 100, 150 and 250 nm. Using fractal analysis, morphological characteristics of surface films thickness in amorphous state were investigated. The results show that with increasing thickness, surface roughness (RMS) and lateral correlation length (ξ) are decreased. Also, the roughness exponent (α) and growth exponent (β) were determined to be 0.74±0.02 and 0.11±0.02, respectively.