Highly ordered vertically grown zinc oxide nanorods (ZnO NRs) were synthesized on ZnO-coated SiO2/Si substrate using zinc acetylacetonate hydrate as a precursor via a simple hydrothermal method at 85 °C. We used 0.05 M of ZnO solution to facilitate the growth of ZnO NRs and the immersion time was varied from 0.5 to 4 h. The atomic force microscopy revealed the surface roughness of ZnO seed layer used to grow the ZnO NRs. The morphology of vertically grown ZnO NRs was observed by field emission scanning electron microscopy. X-ray diffraction examination and transmission electron microscopy confirmed that the structure of highly ordered ZnO NRs was crystalline with a strong (002) peak corresponded to ZnO hexagonal wurtzite structure. The growth of highly ordered ZnO NRs was favorable due to the continuous supply of Zn2+ ions and chelating agents properties obtained from the acetylacetonate-derived precursor during the synthesis. Two-point probe current-voltage measurement and UV-vis spectroscopy of the ZnO NRs indicated a resistivity and optical bandgap value of 0.44 Ω.cm and 3.35 eV, respectively. The photoluminescence spectrum showed a broad peak centered at 623 nm in the visible region corresponded to the oxygen vacancies from the ZnO NRs. This study demonstrates that acetylacetonate-derived precursors can be used for the production of ZnO NRs-based devices with a potential application in biosensors.
Microstructural, topology, inner morphology, and gas-sensitivity of mixed xWO(3)(1-x)Y(2)O(3) nanoparticles (x = 1, 0.95, 0.9, 0.85, 0.8) thick-film semiconductor gas sensors were studied. The surface topography and inner morphological properties of the mixed powder and sensing film were characterized with X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Also, gas sensitivity properties of the printed films were evaluated in the presence of methane (CH(4)) and butane (C(4)H(10)) at up to 500 °C operating temperature of the sensor. The results show that the doping agent can modify some structural properties and gas sensitivity of the mixed powder.
An enhanced ferromagnetic property, visible light active TiO(2) photocatalyst was successfully synthesized by supporting strontium ferrite (SrFe(12)O(19)) onto TiO(2) doped with nitrogen (N) and compared with N-doped TiO(2). The synthesized catalysts were further characterized with X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDS), BET surface area analysis, vibrating sample magnetometer (VSM), X-ray photon spectroscopy (XPS) and visible light spectroscopy analysis for their respective properties. The XRD and EDS revealed the structural and inorganic composition of N-TiO(2) supported on SrFe(12)O(19). The supported N-TiO(2) exhibited a strong ferromagnetic property with tremendous stability against magnetic property losses. It also resulted in reduced band gap (2.8 eV) and better visible light absorption between 400 and 800 nm compared to N-doped TiO(2). The photocatalytic activity was investigated with a recalcitrant phenolic compound namely 2,4-dichlorophenol (2,4-DCP) as a model pollutant under direct bright and diffuse sunlight exposure. A complete degradation of 2,4-DCP was achieved with an initial concentration of 50mg/L for both photocatalysts in 180 min and 270 min respectively under bright sunlight. Similarly the diffuse sunlight study resulted in complete degradation for supported N-TiO(2) and >85% degradation N-TiO(2), respectively. Finally the supported photocatalyst was separated under permanent magnetic field with a mass recovery ≈ 98% for further reuse.
This work investigates the structural formation and analyses of titania membranes (TM) prepared using different vacuum exposure times for molecular weight (MW) cut-off performance and oil/water separation. Titania membranes were synthesized via a sol-gel method and coated on macroporous alumina tubes followed by exposure to a vacuum between 30 and 1200 s and then calcined at 400 °C. X-ray diffraction and nitrogen adsorption analyses showed that the crystallite size and particle size of titania increased as a function of vacuum time. All the TM membranes were mesoporous with an average pore diameter of ~3.6 nm with an anatase crystal morphology. Water, glucose, sucrose, and polyvinylpyrrolidone with 40 and 360 kDa (PVP-40 kDa and PVP-360 kDa) were used as feed solutions for MW cut-off and hexadecane solution for oil filtration investigation. The TM membranes were not able to separate glucose and sucrose, thus indicating the membrane pore sizes are larger than the kinetic diameter of sucrose of 0.9 nm, irrespective of vacuum exposure time. They also showed only moderate rejection (20%) of the smaller PVP-40 kDa, however, all the membranes were able to obtain an excellent rejection of near 100% for the larger PVP-360 kDa molecule. Furthermore, the TM membranes were tested for the separation of oil emulsions with a high concentration of oil (3000 ppm), reaching high oil rejections of more than 90% of oil. In general, the water fluxes increased with the vacuum exposure time indicating a pore structural tailoring effect. It is therefore proposed that a mechanism of pore size tailoring was formed by an interconnected network of Ti-O-Ti nanoparticles with inter-particle voids, which increased as TiO₂ nanoparticle size increased as a function of vacuum exposure time, and thus reduced the water transport resistance through the TM membranes.
Geobacillus zalihae sp. nov., which produces a putative thermostable lipase, represents a novel species, with type strain T1. The characterisation of this intrinsically thermostable T1 lipase either physicochemically or structurally is an important task. The crystallisation of T1lipase in space was carried out using a High-Density Protein Crystal Growth (HDPCG) apparatus with the vapour diffusion method, and X-ray diffraction data were collected. The microgravity environment has improved the size and quality of the crystals as compared to earth grown crystal. The effect of microgravity on the crystallisation of T1 lipase was clearly evidenced by the finer atomic details at 1.35 A resolution. Better electron densities were observed overall compared with the Earth-grown crystals, and comparison shows the subtle but distinct conformations around Na(+) ion binding site stabilized via cation-π interactions. This approach could be useful for solving structure and function of lipases towards exploiting its potentials to various industrial applications.
This present study was conducted to produce defatted oil palm shell (OPS) nanoparticles. Wherein, the OPS nanoparticles
were defatted by solvent extraction method. Several analytical methods including transmission electron microscope (TEM),
X-ray diffraction (XRD), particle size analyzer, scanning electron microscope (SEM), SEM energy dispersive X-ray (SEM-EDX)
and thermal gravimetric analyzer (TGA) were used to characterize the untreated and defatted OPS nanoparticles. It was
found that 75.3% OPS particles were converted into nanoparticles during ball milling. The obtained OPS nanoparticles had
smaller surface area with angular, irregular and crushed shapes under SEM view. The defatted OPS nanoparticles did not
show any agglomeration during TEM observation. However, the untreated OPS nanoparticles had higher decomposition
temperature as compared to the defatted OPS nanoparticles. Based on the characterization results of the OPS nanoparticles,
it is evident that the defatted OPS nanoparticles has the potentiality to be used as filler in biocomposites
Oil palm empty fruit bunch (OPEFB) fibre is widely available in Southeast Asian countries and found to have 60% (w/w) sugar components. OPEFB was pretreated using the ammonia fibre expansion (AFEX) method and characterised physically by the Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy. The results show that there were significant structural changes in OPEFB after the pretreatment step, and the sugar yield after enzymatic hydrolysis using a cocktail of Cellic Ctec2® and Cellic Htec2® increased from 0.15gg(-1) of OPEFB in the raw untreated OPEFB sample to 0.53gg(-1) of OPEFB in AFEX-pretreated OPEFB (i.e. almost a fourfold increase in sugar conversion), which enhances the economic value of OPEFB. A biohydrogen fermentability test of this hydrolysate was carried out using a locally isolated bacterium, Enterobacter sp. KBH6958. The biohydrogen yield after 72h of fermentation was 1.68mol H2 per mol sugar. Butyrate, ethanol, and acetate were the major metabolites.
The aim was to explore the utilization of tea leaf waste fibers (TLWF) as a source for the production of cellulose nanocrystals (CNC). TLWF was first treated with alkaline, followed by bleaching before being hydrolyzed with concentrated sulfuric acid. The materials attained after each step of chemical treatments were characterized and their chemical compositions were studied. The structure analysis was examined by Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). From FTIR analysis, two peaks at 1716 and 1207 cm-1-which represent C=O stretching and C⁻O stretching, respectively-disappeared in the spectra after the alkaline and bleaching treatments indicated that hemicellulose and lignin were almost entirely discarded from the fiber. The surface morphology of TLWF before and after chemical treatments was investigated by scanning electron microscopy (SEM) while the dimension of CNC was determined by transmission electron microscopy (TEM). The extraction of CNC increased the surface roughness and the crystallinity index of fiber from 41.5% to 83.1%. Morphological characterization from TEM revealed the appearance of needle-like shaped CNCs with average diameter of 7.97 nm. The promising results from all the analyses justify TLWF as a principal source of natural materials which can produce CNC.
The ambient sonocatalytic degradation of congo red, methyl orange, and methylene blue by titanium dioxide (TiO(2)) catalyst at initial concentrations between 10 and 50mg/L, catalyst loadings between 1.0 and 3.0mg/L and hydrogen peroxide (H(2)O(2)) concentrations up to 600 mg/L is reported. A 20 kHz ultrasonic processor at 50 W was used to accelerate the reaction. The catalysts were exposed to heat treatments between 400 and 1000 degrees C for up to 4h to induce phase change. Sonocatalysts with small amount of rutile phase showed better sonocatalytic activity but excessive rutile phase should be avoided. TiO(2) heated to 800 degrees C for 2h showed the highest sonocatalytic activity and the degradation of dyes was influenced by their chemical structures, chemical phases and characteristics of the catalysts. Congo red exhibited the highest degradation rate, attributed to multiple labile azo bonds to cause highest reactivity with the free radicals generated. An initial concentration of 10mg/L, 1.5 g/L of catalyst loading and 450 ppm of H(2)O(2) gave the best congo red removal efficiency of above 80% in 180 min. Rate coefficients for the sonocatalytic process was successfully established and the reused catalyst showed an activity drop by merely 10%.
The effect of incorporating different loadings of oil palm bio-ash nanoparticles from agriculture waste on the properties of phenol-formaldehyde resin was investigated in this study. The bio-ash filler was used to enhance the performance of phenol-formaldehyde nanocomposites. Phenol-formaldehyde resin filled with oil palm bio-ash nanoparticles was prepared via the in-situ polymerization process to produce nanocomposites. The transmission electron microscope and particle size analyzer result revealed that oil palm bio-ash nanoparticles had a spherical geometry of 90 nm. Furthermore, X-ray diffraction results confirmed the formation of crystalline structure in oil palm bio-ash nanoparticles and phenol-formaldehyde nanocomposites. The thermogravimetric analysis indicated that the presence of oil palm bio-ash nanoparticles enhanced the thermal stability of the nanocomposites. The presence of oil palm bio-ash nanoparticles with 1% loading in phenol-formaldehyde resin enhanced the internal bonding strength of plywood composites. The scanning electron microscope image revealed that phenol-formaldehyde nanocomposites morphology had better uniform distribution and dispersion with 1% oil palm bio-ash nanoparticle loading than other phenol-formaldehyde nanocomposites produced. The nanocomposite has potential use in the development of particle and panel board for industrial applications.
A modified hydrophilic penta-bismuth hepta-oxide nitrate (Bi5O7NO3) surface was synthesized via a precipitation method using TiO2 and Ag as modified agents. The synthesized product was characterized by different analytical techniques. The removal efficiency was evaluated using mono- and di-sulphonated azo dyes as model pollutants. Different kinetic, isotherm and diffusion models were chosen to describe the adsorption process. X-ray photoelectron spectroscopy (XPS) results revealed no noticeable differences in the chemical states of modified adsorbent when compared to pure Bi5O7NO3; however, the presence of hydrophilic centres such as TiO2 and Ag developed positively charged surface groups and improved its adsorption performance to a wide range of azo dyes. Dyes removal was found to be a function of adsorbent dosage, initial dye concentration, solution pH and temperature. The reduction of Langmuir 1,2-mixed order kinetics to the second or first-order kinetics could be successfully used to describe the adsorption of dyes onto the modified adsorbent. Mass transfer can be described by intra-particle diffusion at a certain stage, but it was not the rate limiting step that controlled the adsorption process. Homogenous behavior of adsorbent surface can be explored by applying Langmuir isotherm to fit the adsorption data.
MWCNTs/TiO2 nanocomposite was prepared by oxidising MWCNT in H2SO4/HNO3 then decorating it with TiO2-p25 nanopowder. The composites were characterised using XRD, TEM, FT-IR PL and UV-vis spectroscopy. The TEM images have shown TiO2 nanoparticles immobilised onto the sidewalls of the MWCNTs. The UV-vis spectrum confirms that the nanocomposites can significantly absorb more light in the visible regions compared with the commercial TiO2 (P25). The catalytic activity of these nanocomposites was determined by photooxidation of MB aqueous solution in the presence of visible light. The MWCNTs/TiO2 (1:3) mass ratio showed maximum degradation efficiency. However, its activity was more favourable in alkaline and a neutral pH than an acidic medium.
Ultraviolet (UV) photodetectors (PDs) based on high-quality well-aligned ZnO nanorods (NRs) were fabricated using both modified and conventional chemical bath deposition (CBD) methods. The modified chemical bath deposition (M-CBD) method was made by adding air bubbles to the growth solution during the CBD process. The viability and effectiveness of M-CBD were examined by developing UV PDs based on ZnO NRs. The ZnO nano-seed layer was coated on a glass substrate utilizing radiofrequency (RF) sputtering. The impact of the different growth-times on morphology, growth rate, crystal structure, and optical and chemical properties were investigated systematically using different characterization techniques, such as field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) analysis, UV-VIS double beam spectrometer, and energy dispersive X-ray analysis (EDX), respectively. The Al/ZnO UV PDs based on ZnO nanorods were fabricated with optimum growth conditions through the two methods of preparation. This study showed that the synthesized ZnO NRs using the M-CBD method for different growth times possess better properties than the conventional method under similar deposition conditions. Despite having the highest aspect ratio and growth rate of ZnO NRs, which were found at 4 h growth duration for both methods, the aspect ratio of ZnO NRs using the M-CBD technique was comparatively higher than the conventional CBD method. Besides, the UV PDs fabricated by the M-CBD method at 5 V bias voltage showed high sensitivity, short response time, quick recovery time, high gain, low dark current, and high photocurrent compared with the UV PD device fabricated by the conventional CBD method.
Iron and 4-(methylamino)benzoic acid have been successfully incorporated into silica extracted from rice husk. The silica/Fe/amine complex, RH-Fe(5% amine), showed a ca. 24% increase in specific surface area compared to RH-Fe. This increase was attributed to the templated formation of regular pores. The XRD showed the RH-Fe(5% amine) to be amorphous. The Friedel-Crafts benzylation reaction with toluene using RH-Fe(5% amine) showed a drastic reduction in the di-substituted products to ca. 1.0%.
Silica supported iron catalyst was prepared from rice husk ash (RHA) via the sol-gel technique using an aqueous solution of iron(III) salt in 3.0 M HNO3. The sample was dried at 110 degrees C and labeled as RHA-Fe. A sample of RHA-Fe was calcined at 700 degrees C for 5 h and labeled as RHA-Fe700. X-ray diffraction spectrogram showed that both RHA-Fe and RHA-Fe700 were amorphous. The SEM/EDX results showed that the metal was present as agglomerates and the Fe ions were not homogeneously distributed in RHA-Fe but RHA-Fe700 was shown to be homogeneous. The specific surface areas for RHA-Fe and RHA-Fe700 were determined by BET nitrogen adsorption studies and found to be 87.4 and 55.8 m(2) g(-1), respectively. Both catalysts showed high activity in the reaction between toluene and benzyl chloride. The mono-substituted benzyltoluene was the major product and both catalysts yielded more than 92% of the product. The GC showed that both the ortho- and para-substituted monoisomers were present in about equal quantities. The minor products consisting of 16 di-substituted isomers were also observed in the GC-MS spectra of both catalytic products. The catalyst was found to be reusable without loss of activity and with no leaching of the metal.
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.
In this study, the unaffected, affected and heavily affected teeth were studied by using X-Ray diffraction method. The D-values, which are related to the crystallite size of the apatite crystals, were calculated according to the Sherrer equation. The crystallite size of unaffected enamel was found to be 1530.95Å, while the affected enamel was 1490.22Å and the heavily affected enamel was 1484.16Å respectively. This study showed that the unaffected enamel has greater crystallite size as compared to the affected and heavily affected enamel.
The identification, characterization and quantification of crystal forms are becoming increasingly important within the pharmaceutical industry. A combination of different physical analytical techniques is usually necessary for this task. In this work solid-state techniques, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and X-ray powder diffractometry (XRPD) were combined to analyze polymorphic purity of crystalline ranitidine-HCl, an antiulcer drug, H2 receptor antagonists. A series of 12 different mixtures of Form 1 and 2 was prepared by geometric mixing and their DRIFT spectra and XRD powder patterns were obtained and analyzed, either alone or combined together, using Artificial Neural Networks (ANNs). A standard feed-forward network, with back-propagation rule and with multi layer perceptron architecture (MPL) was chosen. A working range of 1.0-100% (w/w) of crystal Form 2 in Form 1 was established with a minimum quantifiable level (MQL) of 5.2% and limit of detection of 1.5% (w/w). The results demonstrate that DRIFTS combined with XRPD may be successfully used to distinguish between the ranitidine-HCl polymorphs and to quantify the composition of binary mixtures of the two.
Ultrahigh-molecular-weight polyethylene/high-density polyethylene (UHMWPE/HDPE) blends prepared using polyethylene glycol PEG as the processing aid and hydroxyapatite (HA) as the reinforcing filler were found to be highly processable using conventional melt blending technique. It was demonstrated that PEG reduced the melt viscosity of UHMWPE/HDPE blend significantly, thus improving the extrudability. The mechanical and bioactive properties were improved with incorporation of HA. Inclusion of HA from 10 to 50 phr resulted in a progressive increase in flexural strength and modulus of the composites. The strength increment is due to the improvement on surface contact between the irregular shape of HA and polymer matrix by formation of mechanical interlock. The HA particles were homogenously distributed even at higher percentage showed improvement in wetting ability between the polymer matrix and HA. The inclusion of HA enhanced the bioactivity properties of the composite by the formation of calcium phosphate (Ca-P) precipitates on the composite surface as proven from SEM and XRD analysis.
Polyimide/SiO(2) composite films were prepared from tetraethoxysilane (TEOS) and poly(amic acid) (PAA) based on aromatic diamine (4-aminophenyl sulfone) (4-APS) and aromatic dianhydride (3,3,4,4-benzophenonetetracarboxylic dianhydride) (BTDA) via a sol-gel process in N-methyl-2-pyrrolidinone (NMP). The prepared polyimide/SiO(2) composite films were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and thermogravimetric analysis (TGA). The FTIR results confirmed the synthesis of polyimide (4-APS/BTDA) and the formation of SiO(2) particles in the polyimide matrix. Meanwhile, the SEM images showed that the SiO(2) particles were well dispersed in the polyimide matrix. Thermal stability and kinetic parameters of the degradation processes for the prepared polyimide/SiO(2) composite films were investigated using TGA in N(2) atmosphere. The activation energy of the solid-state process was calculated using Flynn-Wall-Ozawa's method without the knowledge of the reaction mechanism. The results indicated that thermal stability and the values of the calculated activation energies increased with the increase of the TEOS loading and the activation energy also varied with the percentage of weight loss for all compositions.