In recent years, there are increasing interest on applying ultrasonic irradiation for the synthesis of zeolite due to its advantages including remarkable shortened synthesis duration. In this project, the potential of ultrasonic irradiation treatment on the synthesis of zeolite RHO was investigated. Ultrasonic irradiation treatment time was varied from 30 to 120 minutes for the synthesis of zeolite RHO. The zeolite RHO solid samples were characterized with X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA) and nitrogen adsorption-desorption analysis. The application of ultrasonic irradiation treatment in this study has accelerated the synthesis of zeolite RHO where the synthesis duration has been significantly shortened to 2 days compared to 8 days required by conventional hydrothermal heating without ultrasonic irradiation treatment. Highly crystalline zeolite RHO crystals in truncated octahedron morphology were successfully formed.
This paper reports the post-processing ageing phenomena of thermoplastic sago starch (TPS) and plasticised sago pith waste (SPW), which were processed using twin-screw extrusion and compression moulding techniques. Wide angle X-ray diffraction (XRD) analyses showed that after processing, starch molecules rearranged into VH-type (which was formed rapidly right post processing and concluded within 4 days) and B-type (which was formed slowly over a period of months) crystallites. Evidence from Fourier transform infrared spectroscopy (FTIR) analyses corroborated the 2-stage crystallisation process, which observed changes in peak styles and peak intensities (at 1043 and 1026 cm-1) and bandnarrowing. Thermogravimetric analysis (TGA) studies showed that the thermal stability of plasticised SPW declined continuously for 90 days before gradual increments ensued. For all formulations tested, post-processing ageing led to drastic changes in the tensile strength (increased) and elongation at break (decreased). Glycerol and fibres restrained the retrogradation of starch molecules in TPS and SPW.
Cellulose was extracted from kenaf core pulp (KCP) by a series of bleaching processes (D) and alkali treatment (E) in the sequence of (DEED) and pretreated with acid hydrolysis in room temperature for 6 hours. The pretreated and non-treated cellulose were dissolved in lithium hydroxide/urea (LiOH/urea) and subsequently used to produce cellulose membrane cross linked with various percentages of glyoxal from 2.5 to 20%. The effects of acid hydrolysis pretreatment on solubility, crystallinity and morphology were investigated. The acid hydrolysis pretreatment leads to higher solubility of the cellulose solution. The formation of cellulose II and crystallinity index of the cellulose membrane were examined by X-ray diffraction (XRD). Cellulose membrane without acid hydrolysis pretreatment cross linked with higher percentage of glyoxal has higher tensile strength compared with the treated cellulose.
In this study, nano- and microsized zinc oxide (ZnO) materials were doped with different manganese (Mn) contents (1-5 mol%) via a simple sol-gel method. The structural, morphological, optical and chemical environments of the materials were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), UV-visible spectroscopy (UV-vis) and X-ray photoelectron spectroscopy (XPS). XRD results revealed that all synthesised materials were pure and single phased with a hexagonal wurtzite structure of ZnO. However, at a low annealing temperature, a nanorod-like shape can be obtained for all Zn(1-x)MnxO materials. In addition, EDX spectra confirmed the presence of Mn in the ZnO lattice and the atomic percentage was nearly equal to the calculated stoichiometry. UV-vis spectroscopy further revealed that materials in nano size exhibited band gap widening with an increase of the Mn content in the ZnO lattice. In contrast, micron state materials exhibited band gap narrowing with increasing Mn content up to 3% and then begin to widen when Mn > 3%. This is because the band gaps of these materials are affected by the dimensions of the crystals and the Mn content in the materials. Furthermore, XPS results revealed the existence of multiple states of Mn in all synthesised materials. By combining the information obtained from UV-vis and the XPS valence band, shifting in the valence band maximum (VBM) and conduction band minimum (CBM) was observed. Based on XPS results, the calculation of density functional theory studies revealed that the presence of Mn2+, Mn3+, and Mn4+ ions in the materials influences the band gap changes. It was also revealed that the nanosized Zn0.99Mn0.01O exhibited a higher photocatalytic activity than the other samples for degrading methylene blue (MB) dyes, owing to its smallest crystallite size.
In this study, the impact of different oxidizing agents on the structural integrity of activated carbon (AC) and multiwalled carbon nanotubes (MWCNTs) was studied for the removal of BTX from aqueous solution. Seven different combinations of green oxidizing agents (mild organic acids) in conjugation with NaOCl (basic oxidizing agent) were used. The modified adsorbents were analyzed by Brunauer, Emmett, and Teller (BET) surface area analyzer, Fourier transform infrared spectroscopy (FTIR), Boehm titration, Raman spectroscopy, thermal gravimetric analysis (TGA), x-ray diffraction (XRD), zeta potential, and variable pressure field emission scanning electron microscope (VPFESEM). The results suggested that the carbonaceous sorbents modified with combination of citric acid tartaric acid, malic acid and salicylic acid (CTMS-I) showed increased surface area (O-AC: 871.67 m2/g, O-MWCNTs: 336.37 m2/g) and total pore volume (O-AC: 0.59 cm3/g, O-MWCNTs: 0.04 cm3/g), with the significantly improved thermal stability. Preliminary batch adsorption experiments conducted using the present prepared O-AC and O-MWCNTs, showed an improved performance towards the adsorption of BTX, compared with other available reported adsorbents in the literature.
Nanoparticles (NPs) are, frequently, being utilized in multi-dimensional enterprises. Silver nanoparticles (AgNPs) have attracted researchers in the last decade due to their exceptional efficacy at very low volume and stability at higher temperatures. Due to certain limitations of the chemical method of synthesis, AgNPs can be obtained by physical methods including sun rays, microwaves and ultraviolet (UV) radiation. In the current study, the synthesis of pullulan mediated silver nanoparticles (P-AgNPs) was achieved through ultraviolet (UV) irradiation, with a wavelength of 365 nm, for 96 h. P-AgNPs were formed after 24 h of UV-irradiation time and expressed spectra maxima as 415 nm, after 96 h, in UV-vis spectroscopy. The crystallographic structure was "face centered cubic (fcc)" as confirmed by powder X-ray diffraction (PXRD). Furthermore, high resolution transmission electron microscopy (HRTEM) proved that P-AgNPs were covered with a thin layer of pullulan, with a mean crystalline size of 6.02 ± 2.37. The average lattice fringe spacing of nanoparticles was confirmed as 0.235 nm with quasi-spherical characteristics, by selected area electron diffraction (SAED) analysis. These green synthesized P-AgNPs can be utilized efficiently, as an active food and meat preservative, when incorporated into the edible films.
This study presents the electromagnetic (EM) characterization of a multiwalled carbon nanotubes (MWCNT)-silver nanoparticles (AgNP)-reinforced poly(vinyl alcohol) (PVA) hybrid nanocomposite fabricated via the solution mixing technique. Primarily, the structure and morphological properties of the PVA/MWCNT-AgNP hybrid nanocomposite are confirmed by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The complex permittivity (ε*) and permeability (μ*), as well as the electromagnetic scattering parameters are measured using a PNA network analyzer equipped with X-band waveguide. The results showed an enhanced permittivity (ε' ≈ 25) value of the hybrid nanocomposite in the frequency range of 8-12 GHz. However, the permeability decreased to almost zero (μ' ≈ 0.4) since the inclusion of AgNP with an average particle size of 40 nm is not susceptible to magnetization and causes higher magnetic losses (tan δμ) than dielectric losses (tan δε). Remarkably, the hybrid nanocomposite reduced transmission of electromagnetic (EM) wave by nearly 60% in comparison to PVA/MWCNT. This is attributed to the enhanced absorption and reflection at the nanotubes, and metal-dielectric interfaces have induced multiple internal reflections owing to the porous structure of the nanocomposite. The prospect of the PVA/MWCNT-AgNP hybrid nanocomposite is favorable as a thin absorbing material for EM shielding applications.
Welding parameters obviously determine the joint quality during the resistance spot welding process. This study aimed to investigate the effect of welding current and electrode force on the heat input and the physical and mechanical properties of a SS316L and Ti6Al4V joint with an aluminum interlayer. The weld current values used in this study were 11, 12, and 13 kA, while the electrode force values were 3, 4, and 5 kN. Welding time and holding time remained constant at 30 cycles. The study revealed that, as the welding current and electrode force increased, the generated heat input increased significantly. The highest tensile-shear load was recorded at 8.71 kN using 11 kA of weld current and 3 kN of electrode force. The physical properties examined the formation of a brittle fracture and several weld defects on the high current welded joint. The increase in weld current also increased the weld diameter. The microstructure analysis revealed no phase transformation on the SS316L interface; instead, the significant grain growth occurred. The phase transformation has occurred on the Ti6Al4V interface. The intermetallic compound layer was also investigated in detail using the EDX (Energy Dispersive X-Ray) and XRD (X-Ray Diffraction) analyses. It was also found that both stainless steel and titanium alloy have their own fusion zone, which is indicated by the highest microhardness value.
In this work, we report the synthesis and characterization of mixed phase Nb1+xS2 nanoflakes prepared by chemical vapor deposition. The as-grown samples show a high density of flakes (thickness ∼50 nm) that form a continuous film. Raman and X-ray diffraction data show that the samples consist of both 2H and 3R phases, with the 2H phase containing a high concentration of Nb interstitials. These Nb interstitials sit in between the NbS2 layers to form Nb1+xS2. Cross-sectional Energy Dispersive Spectroscopy analysis with transmission electron microscopy suggests that the 2H Nb1+xS2 region is found in thinner flakes, while 3R NbS2 is observed in thicker regions of the films. The evolution of the phase from 2H Nb1+xS2 to 3R NbS2 may be attributed to the change of the growth environment from Nb-rich at the start of the growth to sulfur-rich at the latter stage. It was also found that the incorporation of Nb interstitials is highly dependent on the temperature of the NbCl5 precursor and the position of the substrate in the furnace. Samples grown at high NbCl5 temperature and with substrate located closer to the NbCl5 source show higher incorporation of Nb interstitials. Electrical measurements show linear I-V characteristics, indicating the metallic nature of the Nb1+xS2 film with relatively low resistivity of 4.1 × 10-3Ω cm.
Thermoplastic starch (TPS) hybrid bio-composite films containing microcrystalline cellulose (C) and nano-bentonite (B) as hybrid fillers were studied to replace the conventional non-degradable plastic in packaging applications. Raw oil palm empty fruit bunch (OPEFB) was subjected to chemical treatment and acid hydrolysis to obtain C filler. B filler was ultra-sonicated for better dispersion in the TPS films to improve the filler-matrix interactions. The morphology and structure of fillers were characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). TPS hybrid bio-composite films were produced by the casting method with different ratios of B and C fillers. The best ratio of B/C was determined through the data of the tensile test. FTIR analysis proved the molecular interactions between the TPS and the hybrid fillers due to the presence of polar groups in their structure. XRD analysis confirmed the intercalation of the TPS chains between the B inter-platelets as a result of well-developed interactions between the TPS and hybrid fillers. SEM images suggested that more plastic deformation occurred in the fractured surface of the TPS hybrid bio-composite film due to the higher degree of stretching after being subjected to tensile loading. Overall, the results indicate that incorporating the hybrid B/C fillers could tremendously improve the mechanical properties of the films. The best ratio of B/C in the TPS was found to be 4:1, in which the tensile strength (8.52MPa), Young's modulus (42.0 MPa), elongation at break (116.4%) and tensile toughness of the film were increased by 92%, 146%, 156% and 338%, respectively. The significantly improved strength, modulus, flexibility and toughness of the film indicate the benefits of using the hybrid fillers, since these features are useful for the development of sustainable flexible packaging film.
For highly sensitive pH sensing, an electrolyte insulator semiconductor (EIS) device, based on ZnO nanorod-sensing membrane layers doped with magnesium, was proposed. ZnO nanorod samples prepared via a hydrothermal process with different Mg molar ratios (0-5%) were characterized to explore the impact of magnesium content on the structural and optical characteristics and sensing performance by X-ray diffraction analysis (XRD), atomic force microscopy (AFM), and photoluminescence (PL). The results indicated that the ZnO nanorods doped with 3% Mg had a high hydrogen ion sensitivity (83.77 mV/pH), linearity (96.06%), hysteresis (3 mV), and drift (0.218 mV/h) due to the improved crystalline quality and the surface hydroxyl group role of ZnO. In addition, the detection characteristics varied with the doping concentration and were suitable for developing biomedical detection applications with different detection elements.
Currently the development of green chemistry approach with the use of biomaterial-based activities of microbial cells in the synthesis of various nanostructures has attracted a great attention. In this study, we report on the use of bacterium, Bacillus cereus as a biotemplating agent for the formation of zinc oxide nanoparticles with raspberry- and plate-like structures through a simple thermal decomposition of zinc acetate by maintaining the original pH of the reaction mixtures. Possible mechanism on the formation of the nanostructures is proposed based on the surface chemistry and biochemistry processes involved organic-inorganic interactions between zinc oxide and the microbial cells.
In the present study black tea extract (BTE) solution which is familiar for drinking was used to prepare cerium metal-complexes (Ce(III)-complex). The prepared Ce(III)-complex was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and UV-Vis spectroscopy. The results indicate that BTE solution is a novel green coordination chemistry approach for the synthesis of metal complexes. The outcomes signify that coordination occurs between cerium cations and polyphenols. The synthesis of metal-complexes with superior absorption performance in the visible region is a challenge for optoelectronic device applications. The suspended Ce(III)-complex in distilled water was mixed with poly (vinyl alcohol) (PVA) polymer to fabricate PVA/ Ce(III)-complex composites with controlled optical properties. The PVA/Ce(III)-complexes composite films were characterized by FTIR, XRD, and UV-Vis spectroscopy. The XRD findings confirms the amorphous structure for the synthesized Ce(III)-complexes. The addition of Ce(III)-complex into the PVA host polymer led to the growth of polymer composites with controllable small optical band gaps. It is shown by the FTIR spectra of the composite films that the functional groups of the host PVA have a vigorous interaction with the Ce(III)-complex. The XRD deconvolution on PVA composites reveals the amorphous phase enlargement with increasing Ce(III)-complex concentration. It is indicated in the atomic force microscopy (AFM) that the surface roughness in the doped PVA films increases with the increase of the Ce(III)-complex. There is a decrease in absorption edge from 5.7 to 1.7 eV. It becomes possible to recognize the type of electron transition by studying both the Tauc's model and optical dielectric loss (ɛi) parameter.
In this work, plasticized polymer electrolyte films consisting of chitosan, ammonium nitrate (NH4NO3) and glycerol for utilization in energy storage devices was presented. Various microscopic, spectroscopic and electrochemical techniques were used to characterize the concerned electrolyte and the electrical double-layer capacitor (EDLC) assembly. The nature of complexation between the polymer electrolyte components was examined via X-ray diffraction analysis. In the morphological study, field emission scanning electron microscopy (FESEM) was used to investigate the impact of glycerol as a plasticizer on the morphology of films. The polymer electrolyte (conducting membrane) was found to have a conductivity of 3.21 × 10-3 S/cm. It is indicated that the number density (n), mobility (μ) and diffusion coefficient (D) of ions are increased with the glycerol amount. The mechanism of charge storing was clarified, which implies a non-Faradaic process. The voltage window of the polymer electrolyte is 2.32 V. It was proved that the ion is responsible for charge-carrying via measuring the transference number (TNM). It was also determined that the internal resistance of the EDLC assembly lay between 39 and 50 Ω. The parameters associated with the EDLC assembly are of great importance and the specific capacitance (Cspe) was determined to be almost constant over 1 to 1000 cycles with an average of 124 F/g. Other decisive parameters were found: energy density (18 Wh/kg) and power density (2700 W/kg).
In this study, ternary composites of polyaniline (PANI) with manganese dioxide (MnO2) nanorods and carbon nanotubes (CNTs) were prepared by employing a hydrothermal methodology and in-situ oxidative polymerization of aniline. The morphological analysis by scanning electron microscopy showed that the MnO2 possessed nanorod like structures in its pristine form, while in the ternary PANI@CNT/MnO2 composite, coating of PANI over CNT/MnO2, rods/tubes were evidently seen. The structural analysis by X-ray diffraction and X-ray photoelectron spectroscopy showed peaks corresponding to MnO2, PANI and CNT, which suggested efficacy of the synthesis methodology. The electrochemical performance in contrast to individual components revealed the enhanced performance of PANI@CNT/MnO2 composite due to the synergistic/additional effect of PANI, CNT and MnO2 compared to pure MnO2, PANI and PANI@CNT. The PANI@CNT/MnO2 ternary composite exhibited an excellent specific capacity of 143.26 C g-1 at a scan rate of 3 mV s-1. The cyclic stability of the supercapattery (PANI@CNT/MnO2/activated carbon)-consisting of a battery type electrode-demonstrated a gradual increase in specific capacity with continuous charge-discharge over ~1000 cycles and showed a cyclic stability of 119% compared to its initial value after 3500 cycles.
Conocarpus fiber is an abundantly available and sustainable cellulosic biomass. With its richness in cellulose content, it is potentially used for manufacturing microcrystalline cellulose (MCC), a cellulose derivative product with versatile industrial applications. In this work, different samples of bleached fiber (CPBLH), alkali-treated fiber (CPAKL), and acid-treated fiber (CPMCC) were produced from Conocarpus through integrated chemical process of bleaching, alkaline cooking, and acid hydrolysis, respectively. Characterizations of samples were carried out with Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX), Fourier Transform Infrared-Ray (FTIR), X-ray Diffraction (XRD), Thermogravimetric (TGA), and Differential Scanning Calorimetry (DSC). From morphology study, the bundle fiber feature of CPBLH disintegrated into micro-size fibrils of CPMCC, showing the amorphous compounds were substantially removed through chemical depolymerization. Meanwhile, the elemental analysis also proved that the traces of impurities such as cations and anions were successfully eliminated from CPMCC. The CPMCC also gave a considerably high yield of 27%, which endowed it with great sustainability in acting as alternative biomass for MCC production. Physicochemical analysis revealed the existence of crystalline cellulose domain in CPMCC had contributed it 75.7% crystallinity. In thermal analysis, CPMCC had stable decomposition behavior comparing to CPBLH and CPAKL fibers. Therefore, Conocarpus fiber could be a promising candidate for extracting MCC with excellent properties in the future.
Zinc oxide eugenol (ZOE) cements are generally made up of 80%-90% ZnO powder while the remaining content consists of eugenol bonding resin. ZnO structure plays a major role in the morphology and mechanical properties of ZOE. In this study, we investigated the effects of different particle sizes/shapes of ZnO particles on the surface and mechanical properties of ZOE. Three samples were prepared namely ZnO-Ax, ZnO-B and ZnO-K. The crystallite sizes calculated from XRD were 37.76 nm (ZnO-Ax), 39.46 nm (ZnO-B) and 42.20 nm (ZnO-K) while the average particle sizes obtained by DLS were 21.11nm (ZnO-Ax), 56.73 nm (ZnO-B) and 2012 nm (ZnO-K). Results revealed that the compressive strengths of ZOE-Ax and ZOE-B were improved by 87.92% and 57.16%, respectively, relative to that of commercial ZOE-K. Vickers hardness test demonstrated that the hardness of ZOE-Ax and ZOE-B also increased by 74.9% and 31.1%, respectively. The ZnO-Ax nanostructure possessed a small average particle size (21.11 nm), a homogeneous size distribution (DLS) and an oxygen-rich surface (from EDS and elemental mapping). Meanwhile, ZnO-B exhibited a slightly larger average particle size of 56.73 nm compared with that of other samples. Sample ZnO-Ax demonstrated the highest compressive strength which was attributed to its large particle surface area (21.11 nm particle size) that provided a large contact area and greater interfacial (or interlock) bonding capability if compared to that of ZnO-K sample (2012 nm particle size).
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.
A halloysite nanotubes⁻polyvinyl alcohol⁻polyvinylpyrrolidone (HNTs⁻PVA⁻PVP) composite has been investigated for a quite long time aiming at improving the physico⁻chemical characterization of HNTs. In this work, HNTs⁻PVA⁻PVP composite were prepared based on a unique procedure characterized by crosslinking two polymers with HNTs. The composite of two polymers were modified by treating HNTs with phosphoric acid (H₃PO₄) and by using malonic acid (MA) as a crosslinker. The composite was also treated by adding the dispersion agent sodium dodecyl sulfate (SDS). The HNTs⁻PVA⁻PVP composite shows better characteristics regarding agglomeration when HNTs is treated in advance by H₃PO₄. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), brunauer⁻emmett⁻teller (BET), size distribution, and atomic force microscopy (AFM) are used to characterize the physio-chemical properties of the composite. FTIR shows additional peaks at 2924.29, 1455.7, and 682.4 cm-1 compared to the neat HNTs due to adding MA. Despite that, the XRD spectra do not show a significant difference, the decrease in peak intensity could be attributed to the addition of semi-crystalline PVA and the amorphous PVP. The images taken by TEM and FESEM show the possible effects of MA on the morphology and internal feature of HNTs⁻PVA⁻PVP composite treated by MA by showing the deformation of the matrix. The BET surface area increased to 121.1 m²/g compared to the neat HNTs at 59.1 m²/g. This result, the second highest recorded result, is considered a breakthrough in enhancing the properties of HNTs⁻PVA⁻PVP composite, and treatment by MA crosslinking may attribute to the size and the number of the pores. The results from these techniques clearly showed that a significant change has occurred for treated HNTs⁻PVA⁻PVP composite where MA was added. The characterization of HNTs⁻PVA⁻PVP composite with and without treating HNTs and using crosslinker may lead to a better understanding of this new composites as a precursor to possible applications in the dentistry field.
Gamma-ray radiation was used as a clean and easy method for turning the physicochemical properties of graphene oxide (GO) in this study. Silane functionalized-GO were synthesized by chemically grafting 3-aminopropyltriethoxysilane (APTES) and 3-glycidyloxypropyltrimethoxysilane (GPTES) onto GO surface using gamma-ray irradiation. This established non-contact process is used to create a reductive medium which is deemed simpler, purer and less harmful compared conventional chemical reduction. The resulting functionalized-GO were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), and Raman spectroscopy. The chemical interaction of silane with the GO surface was confirmed by FT-IR. X-ray diffraction reveals the change in the crystalline phases was due to surface functionalization. Surface defects of the GO due to the introduction of silane mioties was revealed by Raman spectroscopy. Thermogravimetric analysis of the functionalized-GO exhibits a multiple peaks in the temperature range of 200-650 °C which corresponds to the degradation of chemically grafted silane on the GO surface.