Due to similarity in composition to the mineral component of bones and human hard tissues, hydroxyapatite with chemical formula Ca10(PO4)6(OH)2 has been widely used in medical field. Both chicken and duck eggshells are mainly composed of calcium carbonate. An attempt has been made to fabricate nanohydroxyapatite (nHA) by chicken (CES) and duck eggshells (DES) as calcium carbonate source (CaCO3). CES and DES were reacted with diammonium hydrogen [(NH4)2HPO4] solution and subjected to microwave heating at 15 mins. Under the effect of microwave irradiation, nHA was produced directly in the solution and involved in crystallographic transformation. Sample characterization was done using by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM).
Polymer electrolyte membranes based on the natural polymer κ-carrageenan were modified and characterized for application in electrochemical devices. In general, pure κ-carrageenan membranes show a low ionic conductivity. New membranes were developed by chemically modifying κ-carrageenan via phosphorylation to produce O-methylene phosphonic κ-carrageenan (OMPC), which showed enhanced membrane conductivity. The membranes were prepared by a solution casting method. The chemical structure of OMPC samples were characterized using Fourier transform infrared spectroscopy (FTIR), 1H nuclear magnetic resonance (1H NMR) spectroscopy and 31P nuclear magnetic resonance (31P NMR) spectroscopy. The conductivity properties of the membranes were investigated by electrochemical impedance spectroscopy (EIS). The characterization demonstrated that the membranes had been successfully produced. The ionic conductivity of κ-carrageenan and OMPC were 2.79 × 10-6 S cm-1 and 1.54 × 10-5 S cm-1, respectively. The hydrated membranes showed a two orders of magnitude higher ionic conductivity than the dried membranes.
In this study, novel nanocomposite films based on regenerated cellulose/halloysite nanotube (RC/HNT) have been prepared using an environmentally friendly ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) through a simple green method. The structural, morphological, thermal and mechanical properties of the RC/HNT nanocomposites were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR), field emission scanning electron microscopy (FESEM), thermal analysis and tensile strength measurements. The results obtained revealed interactions between the halloysite nanotubes and regenerated cellulose matrix. The thermal stability and mechanical properties of the nanocomposite films, compared with pure regenerated cellulose film, were significantly improved When the halloysite nanotube (HNT) loading was only 2 wt.%, the 20% weight loss temperature (T20) increased 20°C. The Young's modulus increased from 1.8 to 4.1 GPa, while tensile strength increased from 35.30 to 60.50 MPa when 8 wt.% halloysite nanotube (HNT) was incorporated, interestingly without loss of ductility. The nanocomposite films exhibited improved oxygen barrier properties and water absorption resistance compared to regenerated cellulose.
A gas sensor array was developed in a 10 × 10 mm(2) space using Screen Printing and Pulse Laser Ablation Deposition (PLAD) techniques. Heater, electrode, and an insulator interlayer were printed using the screen printing method on an alumina substrate, while tin oxide and platinum films, as sensing and catalyst layers, were deposited on the electrode at room temperature using the PLAD method, respectively. To ablate SnO(2) and Pt targets, depositions were achieved by using a 1,064 nm Nd-YAG laser, with a power of 0.7 J/s, at different deposition times of 2, 5 and 10 min, in an atmosphere containing 0.04 mbar (4 kPa) of O(2). A range of spectroscopic diffraction and real space imaging techniques, SEM, EDX, XRD, and AFM were used in order to characterize the surface morphology, structure, and composition of the films. Measurement on the array shows sensitivity to some solvent and wood smoke can be achieved with short response and recovery times.
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.
Recently, TiO2/multi-walled carbon nanotube (MWCNT) hybrid nanocatalysts have been a subject of high interest due to their excellent structures, large surface areas and peculiar optical properties, which enhance their photocatalytic performance. In this work, a modified microwave technique was used to rapidly synthesise a TiO2/MWCNT nanocatalyst with a large surface area. X-ray powder diffraction, field-emission scanning electron microscopy, transmission electron microscopy and Brunauer-Emmett-Teller measurements were used to characterise the structure, morphology and the surface area of the sample. The photocatalytic activity of the hybrid nanocatalysts was evaluated through a comparison of the degradation of methylene blue dye under irradiation with ultraviolet and visible light. The results showed that the TiO2/MWCNT hybrid nanocatalysts degraded 34.9% of the methylene blue (MB) under irradiation with ultraviolet light, whereas 96.3% of the MB was degraded under irradiation with visible light.
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.
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.
Silver (Ag) coated bioactive glass particles (Ag-BG) were formulated and compared to uncoated controls (BG) in relation to glass characterization, solubility and microbiology. X-ray diffraction (XRD) confirmed a crystalline AgNP surface coating while ion release studies determined low Ag release (<2 mg/L). Cell culture studies presented increased cell viability (127 and 102%) with lower liquid extract (50 and 100 ml/ml) concentrations. Antibacterial testing of Ag-BG in E. coli, S. epidermidis and S. aureus significantly reduced bacterial cell viability by 60-90%. Composites of Ag-BG/CMC-Dex Hydrogels were formulated and characterized. Agar diffusion testing was conducted where Ag-BG/hydrogel composites produced the largest inhibition zones of 7 mm (E. coli), 5 mm (S. aureus) and 4 mm (S. epidermidis).
Co(II)-Ti(IV)-substituted magnetoplumbite-type (M-type) barium ferrite nanoparticles were synthesized via the sol-gel technique employing ethylene glycol as the gel precursor. Structural and magnetic properties were characterised via X-ray diffraction (XRD), high resolution transmission electron microscopy and superconducting quantum interference device magnetometry. The particle sizes of the M-type BaCoXTiXFe12-2XO19 (0.2 ≤ ≤ 1.0) were found to be 900 Å – 1500 Å. The XRD results confirmed that the Co(II)-Ti(IV) substituted ferrites in the range of 0.2 ≤ ≤ 1.0 substitution had the M-type ferrite as the dominant phase. The hysteresis loss per-cycle decreased with increasing Co(II)-Ti(IV) substitution in M-type ferrites which showed reduced values in coercivity and remnant magnetisation with moderate effect on the saturation magnetisation.
Carbonation for the curing of cement-based materials has been gaining increased attention in recent years, especially in light of emerging initiatives to reduce carbon dioxide (CO2) emissions. Carbonation method or CO2 curing is founded on the basis of the reaction between CO2 and cement products to form thermally stable and denser carbonate, which not only improves the physical and mechanical properties of cement-based materials, but also has the ability to utilize and store CO2 safely and permanently. This study aims to assess the effect of CO2 curing technology on the high-temperatures performance of cement blocks. Upon molding, dry-mix cement blocks were cured under statically accelerated carbonation condition (20% CO2 concentration with 70% relative humidity) for 28 days, followed by exposure to elevated temperatures of 300 °C to 800 °C in order to comprehensively study the principal phase changes and decompositions of cement hydrates. The results indicated that CO2 curing improved the performance of cement blocks, such as enhancement in the residual compressive strength and reducing the sorptivity. At 600 °C, the scanning electron microscopy (SEM) revealed a denser microstructure while thermal analisis and X-ray diffraction (XRD) analysis also clearly demonstrated that higher amounts of calcium carbonate were present in the cement blocks after CO2 curing, suggesting better high-temperature performance compared to natural cured cement blocks. In general, an improved high-temperature performance, specifically at 600 °C of the dry-mixed cement blocks was demonstrated by adopting the CO2 curing technology. This confirms the potential of utilizing CO2 curing technology in not only improving quality of cement blocks, new avenue for storing of CO2 in construction material can be realized at the same time.
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.
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.
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.
In this research, silver nanoparticles (AgNPs) were synthesized in chitosan (Cts), Cts/gelatin and gelatin suspensions using a chemical reducing agent. Cts and gelatin were used as natural stabilizers and solid support, whereas AgNO(3) was used as the silver precursor. Sodium borohydride (NaBH(4)) was used as the reducing agent. The properties of AgNPs in Cts, Cts/gelatin and gelatin bionanocomposites (BNCs) were studied in terms of their surface plasmon resonance, crystalline structure, average diameter size, particle distributions, surface topography and functional groups. All the samples were characterized by UV-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, atomic force microscopy and Fourier transform infrared spectroscopy.
ZnO nanostructures were synthesized by hydrothermal method using different molar ratios of cetyltrimethylammonium bromide (CTAB) and Sodium dodecyl sulfate (SDS) as structure directing agents. The effect of surfactants on the morphology of the ZnO crystals was investigated by field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) techniques. The results indicate that the mixture of cationic-anionic surfactants can significantly modify the shape and size of ZnO particles. Various structures such as flakes, sheets, rods, spheres, flowers and triangular-like particles sized from micro to nano were obtained. In order to examine the possible changes in other properties of ZnO, characterizations like powder X-ray diffraction (PXRD), thermogravimetric and differential thermogravimetric analysis (TGA-DTG), FTIR, surface area and porosity and UV-visible spectroscopy analysis were also studied and discussed.
A solution-phase route has been considered as the most promising route to synthesize noble nanostructures. A majority of their synthesis approaches of calcium carbonate (CaCO3) are based on either using fungi or the CO2 bubbling methods. Here, we approached the preparation of nano-precipitated calcium carbonate single crystal from salmacis sphaeroides in the presence of zwitterionic or cationic biosurfactants without external source of CO2. The calcium carbonate crystals were rhombohedron structure and regularly shaped with side dimension ranging from 33-41 nm. The high degree of morphological control of CaCO3 nanocrystals suggested that surfactants are capable of strongly interacting with the CaCO3 surface and control the nucleation and growth direction of calcium carbonate nanocrystals. Finally, the mechanism of formation of nanocrystals in light of proposed routes was also discussed.
Iron-manganese-doped sulfated zirconia nanoparticles with both Lewis and Brønsted acidic sites were prepared by a hydrothermal impregnation method followed by calcination at 650°C for 5 hours, and their cytotoxicity properties against cancer cell lines were determined. The characterization was carried out using X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, Brauner-Emmett-Teller (BET) surface area measurements, X-ray fluorescence, X-ray photoelectron spectroscopy, zeta size potential, and transmission electron microscopy (TEM). The cytotoxicity of iron-manganese-doped sulfated zirconia nanoparticles was determined using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assays against three human cancer cell lines (breast cancer MDA-MB231 cells, colon carcinoma HT29 cells, and hepatocellular carcinoma HepG2 cells) and two normal human cell lines (normal hepatocyte Chang cells and normal human umbilical vein endothelial cells [HUVECs]). The results suggest for the first time that iron-manganese-doped sulfated zirconia nanoparticles are cytotoxic to MDA-MB231 and HepG2 cancer cells but have less toxicity to HT29 and normal cells at concentrations from 7.8 μg/mL to 500 μg/mL. The morphology of the treated cells was also studied, and the results supported those from the cytotoxicity study in that the nanoparticle-treated HepG2 and MDA-MB231 cells had more dramatic changes in cell morphology than the HT29 cells. In this manner, this study provides the first evidence that iron-manganese-doped sulfated zirconia nanoparticles should be further studied for a wide range of cancer applications without detrimental effects on healthy cell functions.
Cellulose nanofibers (CNF) isolated from plant biomass have attracted considerable interests in polymer engineering. The limitations associated with CNF-based nanocomposites are often linked to the time-consuming preparation methods and lack of desired surface functionalities. Herein, we demonstrate the feasibility of preparing a multifunctional CNF-zinc oxide (CNF-ZnO) nanocomposite with dual antibacterial and reinforcing properties via a facile and efficient ultrasound route. We characterized and examined the antibacterial and mechanical reinforcement performances of our ultrasonically induced nanocomposite. Based on our electron microscopy analyses, the ZnO deposited onto the nanofibrous network had a flake-like morphology with particle sizes ranging between 21 to 34 nm. pH levels between 8-10 led to the formation of ultrafine ZnO particles with a uniform size distribution. The resultant CNF-ZnO composite showed improved thermal stability compared to pure CNF. The composite showed potent inhibitory activities against Gram-positive (methicillin-resistant Staphylococcus aureus (MRSA)) and Gram-negative Salmonella typhi (S. typhi) bacteria. A CNF-ZnO-reinforced natural rubber (NR/CNF-ZnO) composite film, which was produced via latex mixing and casting methods, exhibited up to 42% improvement in tensile strength compared with the neat NR. The findings of this study suggest that ultrasonically-synthesized palm CNF-ZnO nanocomposites could find potential applications in the biomedical field and in the development of high strength rubber composites.
Samples of Y-Ba-Cu-O superconductor with nominal compositions of YBa2Cu3O7-d + x (weight %) Y2O3 (x = 0 - 15) were prepared by solid state reaction method using the Y2Cu2O5 and BaCuO2 precursors as the starting reagents. The X-ray diffraction (XRD) diffractograms for the doped samples (x> 0) show an additional non-superconducting Y2BaCuO5 (211) phase. The scanning electron microscope (SEM) micrographs show that the smaller Y2BaCuO5 grains are precipitated on the surface of the larger YBa2Cu3O7-d (YBCO) crystals. The grain size of the YBCO decreases with increasing yttria. The superconducting zero resistivity critical temperature (Tco) of the doped samples is very close to the Tco of the YBCO for x < 5, but it seems to be significantly decreasing for larger x. The transport critical current density (J) for x < 5 is enhanced due to magnetic flux pinning process by the 211 phase. However, Jc decreased for larger x due to the increase of weak links at the grain boundaries of the YBCO phase.
Sampel superkonduktor Y-Ba-Cu-O dengan komposisi nominal YBa2Cu3O7-d + x (% berat) Y2O3 (x = 0 -15) disediakan dengan kaedah tindakbalas keadaan pepejal menggunakan bahan pelopor Y2Cu2O5 dan BaCuO2 Difraktogram pembelauan sinar-X (XRD) bagi sampel yang didop (x > 0) menunjukkan wujudnya fasa tak mensuperkonduksi Y2BaCuO5 (211). Mikrograf mikroskop imbasan elektron (SEM) menunjukkan bahawa butiran Y2BaCuO5 yang lebih kecil itu termendap di atas permukaan hablur YBa2Cu3O7-d yang lebih besar. Saiz hablur YBCO mengecil dengan peningkatan yittria. Suhu genting kerintangan sifar (Tc) bagi sampel yang didop adalah hampir dengan Tco bagi YBCO untuk x<5, tetapi menurun dengan agak cepat untuk x yang lebih besar. Ketumpatan arus genting angkutan (J) untuk x < 5 meningkat jika dibandingkan dengan YBCO disebabkan oleh proses kepinan fluks magnet oleh fasa 211. Walau bagaimanapun, Jc menurun untuk x yang lebih tinggi kerana meningkatnya hubungan lemah pada sempadan butiran fasa YBCO.