Chemical structure of treated and untreated Aciplex membrane has been studied by X-ray Photoelectron Spectroscopy (XPS). Survey spectra showed that both membrane surfaces consist of Fluorine, Carbon, Oxygen, Sulphur and trace of Titanium. Binding energies for the elements are (C1s at 290.6 eV, F1s at 687.5 eV, O1s at 531.3 eV, S2P at 168.1 eV and Ti2P at 454.4 eV). Analysis of narrow scan XPS-spectra of each element demonstrate the presence of (-CF, -CF2, CF3, C-O-C and SO-3) groups, which are in agreement with the structural formula as disclosed by the manufacturer. There is no significant change in chemical states of untreated and treated membrane, which reflect its stability to treatment conditions.
Struktur kimia Aciplex membran yang sudah dibersihkan dan yang belum dibersihkan telah dikaji menggunakan Spektroskopi Fotoelektron Sinaran-X (XPS). Spektra yang telah ditinjau menunjukkan bahawa kedua-dua permukaan membran mengandungi Florin, Karbon, Oksigen, Sulfur dan sedikit Titanium. Tenaga ikatan bagi unsur-unsur tersebut adalah (C1s pada 290.6 eV, F1s pada 687.5 eV. O1s pada 531.3 eV, S2P pada 168.2 eV dan Ti2P pada 454.4 eV). Analisis imbasan kecil spektra-xps bagi setiap unsur menunjukkan kehadiran kilmpulan (-CF, - CF2, CF3, C-O-C dan SO-3) yang bertepatan dengan formula struktur dari pihak pembekal. Tiada terdapat perubahan nyata berhubung dengan keadaan kimia membran yang sudah dibersihkan dan yang belum dibersihkan yang menggambarkan kestabilannya terhadap keadaan pembersihan.
The aim of this study was to determine the surface chemistry during biocorrosion process on growth and on the production of exopolymeric substances (EPS) in batch cultures of mix-strains of marine sulphate-reducing bacteria (SRB) isolated from Malaysian Shipyard and Engineering Harbours, Pasir Gudang. The EPS and precipitates were analyzed by x-ray photoelectron spectroscopy (XPS). The XPS results indicate that Fe(2p3/2) spectrum for iron sulphide can be fitted with Fe(II) and Fe(III) components, both corresponding to Fe-S bond types. The absence of oxide oxygen in the O(1s) spectrum and Fe(III)-O bond types in the Fe(2p3/2) spectrum supports the conclusion that iron sulphides are composed of both ferric and ferrous iron coordinated with monosulphide and disulphide.
This review briefly describes some of the techniques available for analysing surfaces and illustrates their usefulness with a few examples such as a metal and alloy. In particular, Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) and laser Raman spectroscopy are all described as advanced surface analytical techniques. In analysing a surface, AES and XPS would normally be considered first, with AES being applied where high spatial resolution is required and XPS where chemical state information is needed. Laser Raman spectroscopy is useful for determining molecular bonding. A combination of XPS, AES and Laser Raman spectroscopy can give quantitative analysis from the top few atomic layers with a lateral spatial resolution of
The present study deals with surface modification of Ti6Al4V alloy via anodization technique. The morphology, structure, adhesion and bioactivity of Ti6Al4V alloy after anodization process were investigated in detail. The influence of fluoride content and direct circuit (DC) applied voltage during anodization of Ti6Al4V alloy in a bath with electrolytes composed of ethylene glycol (EG) and ammonium fluoride (NH4F) were considered. It was found that the average pore sizes and length of nanoporous or nanotubes were increasing with the fluoride content and applied voltage. A minimum of 3 wt% of NH4F is required to grow a self-organized nanotube arrays. As the fluoride content was increased to 5 wt%, TiO2 nanotubes with average diameter of 110 nm and 3.4 microm lengths were successfully synthesized. It is noteworthy to point out that the rate of the nanotube formation was increasing up to 9 microm thick bioactive TiO2 nanotubes layer as anodization time was increased to 3 h. Based on the results obtained, the PA6 cells cultured on anodic Ti6Al4V alloy showed highest level of cell viability and greater cell adhesion compared to the flat Ti6Al4V foil substrate. In fact, highly ordered nanotubes structure on Ti6Al4V alloy can provide beneficial effects for PA6 cells in attachment and proliferation.
The effects of different post-deposition annealing ambients (oxygen, argon, forming gas (95% N2 + 5% H2), and nitrogen) on radio frequency magnetron-sputtered yttrium oxide (Y2O3) films on n-type gallium nitride (GaN) substrate were studied in this work. X-ray photoelectron spectroscopy was utilized to extract the bandgap of Y2O3 and interfacial layer as well as establishing the energy band alignment of Y2O3/interfacial layer/GaN structure. Three different structures of energy band alignment were obtained, and the change of band alignment influenced leakage current density-electrical breakdown field characteristics of the samples subjected to different post-deposition annealing ambients. Of these investigated samples, ability of the sample annealed in O2 ambient to withstand the highest electric breakdown field (approximately 6.6 MV/cm) at 10-6 A/cm2 was related to the largest conduction band offset of interfacial layer/GaN (3.77 eV) and barrier height (3.72 eV).
PtRu catalyst is a promising anodic catalyst for direct methanol fuel cells (DMFCs) but the slow reaction kinetics reduce the performance of DMFCs. Therefore, this study attempts to improve the performance of PtRu catalysts by adding nickel (Ni) and iron (Fe). Multiwalled carbon nanotubes (MWCNTs) are used to increase the active area of the catalyst and to improve the catalyst performance. Electrochemical analysis techniques, such as energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS), are used to characterize the kinetic parameters of the hybrid catalyst. Cyclic voltammetry (CV) is used to investigate the effects of adding Fe and Ni to the catalyst on the reaction kinetics. Additionally, chronoamperometry (CA) tests were conducted to study the long-term performance of the catalyst for catalyzing the methanol oxidation reaction (MOR). The binding energies of the reactants and products are compared to determine the kinetics and potential surface energy for methanol oxidation. The FESEM analysis results indicate that well-dispersed nanoscale (2-5 nm) PtRu particles are formed on the MWCNTs. Finally, PtRuFeNi/MWCNT improves the reaction kinetics of anode catalysts for DMFCs and obtains a mass current of 31 A g(-1) catalyst.
The purpose of this work is to remove Pb(II) from the aqueous solution using a type of hydrogel composite. A hydrogel composite consisting of waste linear low density polyethylene, acrylic acid, starch, and organo-montmorillonite was prepared through emulsion polymerization method. Fourier transform infrared spectroscopy (FTIR), Solid carbon nuclear magnetic resonance spectroscopy (CNMR)), silicon(-29) nuclear magnetic resonance spectroscopy (Si NMR)), and X-ray diffraction spectroscope ((XRD) were applied to characterize the hydrogel composite. The hydrogel composite was then employed as an adsorbent for the removal of Pb(II) from the aqueous solution. The Pb(II)-loaded hydrogel composite was characterized using Fourier transform infrared spectroscopy (FTIR)), scanning electron microscopy (SEM)), and X-ray photoelectron spectroscopy ((XPS)). From XPS results, it was found that the carboxyl and hydroxyl groups of the hydrogel composite participated in the removal of Pb(II). Kinetic studies indicated that the adsorption of Pb(II) followed the pseudo-second-order equation. It was also found that the Langmuir model described the adsorption isotherm better than the Freundlich isotherm. The maximum removal capacity of the hydrogel composite for Pb(II) ions was 430mg/g. Thus, the waste linear low-density polyethylene-g-poly (acrylic acid)-co-starch/organo-montmorillonite hydrogel composite could be a promising Pb(II) adsorbent.
Hybrid gold nanostructures seeded into nanotextured zinc oxide (ZnO) nanoflowers (NFs) were created for novel biosensing applications. The selected 'spotted NFs' had a 30-nm-thick gold nanoparticle (AuNP) layer, chosen from a range of AuNP thicknesses, sputtered onto the surface. The generated nanohybrids, characterized by morphological, physical and structural analyses, were uniformly AuNP-seeded onto the ZnO NFs with an average length of 2-3 μm. Selective capture of molecular probes onto the seeded AuNPs was evidence for the specific interaction with DNA from pathogenic Leptospirosis-causing strains via hybridization and mis-match analyses. The attained detection limit was 100 fM as determined via impedance spectroscopy. High levels of stability, reproducibility and regeneration of the sensor were obtained. Selective DNA immobilization and hybridization were confirmed by nitrogen and phosphorus peaks in an X-ray photoelectron spectroscopy analysis. The created nanostructure hybrids illuminate the mechanism of generating multiple-target, high-performance detection on a single NF platform, which opens a new avenue for array-based medical diagnostics.
Band gap change in doped ZnO is an observed phenomenon that is very interesting from the fundamental point of view. This work is focused on the preparation of pure and single phase nanostructured ZnO and Cu as well as Mn-doped ZnO for the purpose of understanding the mechanisms of band gap narrowing in the materials. ZnO, Zn0.99Cu0.01O and Zn0.99Mn0.01O materials were prepared using a wet chemistry method, and X-ray diffraction (XRD) results showed that all samples were pure and single phase. UV-visible spectroscopy showed that materials in the nanostructured state exhibit band gap widening with respect to their micron state while for the doped compounds exhibited band gap narrowing both in the nano and micron states with respect to the pure ZnO materials. The degree of band gap change was dependent on the doped elements and crystallite size. X-ray photoelectron spectroscopy (XPS) revealed that there were shifts in the valence bands. From both UV-visible and XPS spectroscopy, it was found that the mechanism for band gap narrowing was due to the shifting of the valance band maximum and conduction band minimum of the materials. The mechanisms were different for different samples depending on the type of dopant and dimensional length scales of the crystallites.
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.
In this paper, we address the synthesis of nano-coalesced microstructured zinc oxide thin films via a simple thermal evaporation process. The role of synthesis temperature on the structural, morphological, and optical properties of the prepared zinc oxide samples was deeply investigated. The obtained photoluminescence and X-ray photoelectron spectroscopy outcomes will be used to discuss the surface structure defects of the prepared samples. The results indicated that the prepared samples are polycrystalline in nature, and the sample prepared at 700 °C revealed a tremendously c-axis oriented zinc oxide. The temperature-driven morphological evolution of the zinc oxide nano-coalesced microstructures was perceived, resulting in transformation of quasi-mountain chain-like to pyramidal textured zinc oxide with increasing the synthesis temperature. The results also impart that the sample prepared at 500 °C shows a higher percentage of the zinc interstitial and oxygen vacancies. Furthermore, the intensity of the photoluminescence emission in the ultraviolet region was enhanced as the heating temperature increased from 500 °C to 700 °C. Lastly, the growth mechanism of the zinc oxide nano-coalesced microstructures is discussed according to the reaction conditions.
Cobalt titanate-titania composite oxide films have been grown on FTO-coated glass substrates using a single-source heterometallic complex [Co2Ti4(μ-O)6(TFA)8(THF)6]·THF () which was obtained in quantitative yield from the reaction of diacetatocobalt(ii) tetrahydrate, tetraisopropoxytitanium(iv), and trifluoroacetic acid from a tetrahydrofuran solution. Physicochemical investigations of complex have been carried out by melting point, FT-IR, thermogravimetric and single-crystal X-ray diffraction analyses. CoTiO3-TiO2 films composed of spherical objects of various sizes have been grown from by aerosol-assisted chemical vapor deposition at different temperatures of 500, 550 and 600 °C. Thin films characterized by XRD, Raman and X-ray photoelectron spectroscopy, scanning electron microscopy, energy-dispersive X-ray analysis have been explored for electrochemical detection of dopamine (DA). The cyclic voltammetry with the CoTiO3-TiO2 electrode showed a DA oxidation peak at +0.215 V while linear sweep voltammetry displayed a detection limit (LoD) of 0.083 μM and a linear concentration range of 20-300 μM for DA. Thus, the CoTiO3-TiO2 electrode is a potential candidate for the sensitive and selective detection of DA.
In the present study, the construction of arrays on silicon for naked-eye detection of DNA dengue was demonstrated. The array was created by exposing a polyethylene glycol (PEG) silane monolayer to 254 nm ultraviolet (UV) light through a photomask. Formation of the PEG silane monolayer and photomodifed surface properties was thoroughly characterized by using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements. The results of XPS confirmed that irradiation of ultraviolet (UV) light generates an aldehyde functional group that offers conjugation sites of amino DNA probe for detection of a specific dengue virus target DNA. Employing a gold enhancement process after inducing the electrostatic interaction between positively charged gold nanoparticles and the negatively charged target DNA hybridized to the DNA capture probe allowed to visualize the array with naked eye. The developed arrays demonstrated excellent performance in diagnosis of dengue with a detection limit as low as 10 pM. The selectivity of DNA arrays was also examined using a single base mismatch and noncomplementary target DNA.
In this study, we synthesized a multifunctional nanoparticulate system with specific targeting, imaging, and drug delivering functionalities by following a three-step protocol that operates at room temperature and solely in aqueous media. The synthesis involves the encapsulation of luminescent Mn:ZnS quantum dots (QDs) with chitosan not only as a stabilizer in biological environment, but also to further provide active binding sites for the conjugation of other biomolecules. Folic acid was incorporated as targeting agent for the specific targeting of the nanocarrier toward the cells overexpressing folate receptors. Thus, the formed composite emits orange-red fluorescence around 600 nm and investigated to the highest intensity at Mn(2+) doping concentration of 15 at.% and relatively more stable at low acidic and low alkaline pH levels. The structural characteristics and optical properties were thoroughly analyzed by using Fourier transform infrared, X-ray diffraction, dynamic light scattering, ultraviolet-visible, and fluorescence spectroscopy. Further characterization was conducted using thermogravimetric analysis, high-resolution transmission electron microscopy, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray fluorescence, and X-ray photoelectron spectroscopy. The cell viability and proliferation studies by means of MTT assay have demonstrated that the as-synthesized composites do not exhibit any toxicity toward the human breast cell line MCF-10 (noncancer) and the breast cancer cell lines (MCF-7 and MDA-MB-231) up to a 500 µg/mL concentration. The cellular uptake of the nanocomposites was assayed by confocal laser scanning microscope by taking advantage of the conjugated Mn:ZnS QDs as fluorescence makers. The result showed that the functionalization of the chitosan-encapsulated QDs with folic acid enhanced the internalization and binding affinity of the nanocarrier toward folate receptor-overexpressed cells. Therefore, we hypothesized that due to the nontoxic nature of the composite, the as-synthesized nanoparticulate system can be used as a promising candidate for theranostic applications, especially for a simultaneous targeted drug delivery and cellular imaging.
Cs2Pb(MoO4)2crystals were prepared by crystallization from their own melt, and the crystal structure has been studied in detail. At 296 K, the molybdate crystallizes in the low-temperature α-form and has a monoclinic palmierite-related superstructure (space group C2/m, a = 2.13755(13) nm, b = 1.23123(8) nm, c = 1.68024(10) nm, β = 115.037(2)°, Z = 16) possessing the largest unit cell volume, 4.0066(4) nm3, among lead-containing palmierites. The compound undergoes a distortive phase transition at 635 K and incongruently melts at 943 K. The electronic structure of α-Cs2Pb(MoO4)2was explored by using X-ray emission spectroscopy (XES) and X-ray photoelectron spectroscopy methods. For α-Cs2Pb(MoO4)2, the photoelectron core-level and valence-band spectra and the XES band representing the energy distribution of Mo 4d and O 2p states were recorded. Our results allow one to conclude that the Mo 4d and O 2p states contribute mainly to the central part and at the top of the valence band, respectively, with also significant contributions throughout the whole valence-band region of the molybdate under consideration.
The performance of a modified electrode of nanocomposite films consisting of polypyrrole-chitosan-titanium dioxide (Ppy-CS-TiO₂) has been explored for the developing a non-enzymatic glucose biosensors. The synergy effect of TiO₂ nanoparticles (NPs) and conducting polymer on the current responses of the electrode resulted in greater sensitivity. The incorporation of TiO₂ NPs in the nanocomposite films was confirmed by X-ray photoelectron spectroscopy (XPS) spectra. FE-SEM and HR-TEM provided more evidence for the presence of TiO₂ in the Ppy-CS structure. Glucose biosensing properties were determined by amperommetry and cyclic voltammetry (CV). The interfacial properties of nanocomposite electrodes were studied by electrochemical impedance spectroscopy (EIS). The developed biosensors showed good sensitivity over a linear range of 1-14 mM with a detection limit of 614 μM for glucose. The modified electrode with Ppy-CS nanocomposite also exhibited good selectivity and long-term stability with no interference effect. The Ppy-CS-TiO₂ nanocomposites films presented high electron transfer kinetics. This work shows the role of nanomaterials in electrochemical biosensors and describes the process of their homogeneous distribution in composite films by a one-step electrochemical process, where all components are taken in a single solution in the electrochemical cell.
In this study, we propose an innovative, bio-based, environmentally friendly approach for the covalent functionalization of multi-walled carbon nanotubes using clove buds. This approach is innovative because we do not use toxic and hazardous acids which are typically used in common carbon nanomaterial functionalization procedures. The MWCNTs are functionalized in one pot using a free radical grafting reaction. The clove-functionalized MWCNTs (CMWCNTs) are then dispersed in distilled water (DI water), producing a highly stable CMWCNT aqueous suspension. The CMWCNTs are characterized using Raman spectroscopy, X-ray photoelectron spectroscopy and transmission electron microscopy. The electrostatic interactions between the CMWCNT colloidal particles in DI water are verified via zeta potential measurements. UV-vis spectroscopy is also used to examine the stability of the CMWCNTs in the base fluid. The thermo-physical properties of the CMWCNT nano-fluids are examined experimentally and indeed, this nano-fluid shows remarkably improved thermo-physical properties, indicating its superb potential for various thermal applications.
This paper presents a new approach in assembling bone extracellular matrix components onto PLA films, and investigates the most favourable environment which can be created using the technique for cell-material interactions. Poly (lactic acid) (PLA) films were chemically modified by covalently binding the poly(ethylene imine) (PEI) as to prepare the substrate for immobilization of polyelectrolyte multilayers (PEMs) coating. Negatively charged polyelectrolyte consists of well-dispersed silicon-carbonated hydroxyapatite (SiCHA) nanopowders in hyaluronic acid (Hya) was deposited onto the modified PLA films followed by SiCHA in collagen type I as the positively charged polyelectrolyte. The outermost layer was finally cross-linked by 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrocholoride and N-hydroxysulfosuccinimide sodium salt (EDC/NHS) solutions. The physicochemical features of the coated PLA films were monitored via X-ray Photoelectron Spectroscopy (XPS) and Atomic Force Microscope (AFM). The amounts of calcium and collagen deposited on the surface were qualitatively and quantitatively determined. The surface characterizations suggested that 5-BL has the optimum surface roughness and highest amounts of calcium and collagen depositions among tested films. In vitro human mesenchymal stem cells (hMSCs) cultured on the coated PLA films confirmed that the coating materials greatly improved cell attachment and survival compared to unmodified PLA films. The cell viability, cell proliferation and Alkaline Phosphatase (ALP) expression on 5-BL were found to be the most favourable of the tested films. Hence, this newly developed coating materials assembly could contribute to the improvement of the bioactivity of polymeric materials and structures aimed to bone tissue engineering applications.
Acanthamoeba species are pathogenic protozoa which account for amoebic keratitis, conjunctivitis and granulomatous amoebic encephalitis. These amoebae form cysts which resist drugs and more effective acanthamoebicidal agents are needed. Medicinal plants could be useful in improving the current treatment strategies for Acanthamoeba infections. In the present study, we examined the amoebicidal effects of Pericampylus glaucus (Lam.) Merr., a medicinal plant used for the treatment of conjunctivitis in Malaysia. Pathogenic Acanthamoeba triangularis were isolated from environmental water samples and treated with different concentrations of fractions obtained from Pericampylus glaucus (Lam.) Merr. as well as main constituents for 24-72 h. Chlorhexidine was used as a reference drug. Ethanol fraction of stem showed significant (p
In the present study, binary oxide (cadmium oxide [CdO])x (zinc oxide [ZnO])1-x nanoparticles (NPs) at different concentrations of precursor in calcination temperature were prepared using thermal treatment technique. Cadmium and zinc nitrates (source of cadmium and zinc) with polyvinylpyrrolidone (capping agent) have been used to prepare (CdO)x (ZnO)1-x NPs samples. The sample was characterized by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. XRD patterns analysis revealed that NPs were formed after calcination, which showed a cubic and hexagonal crystalline structure of (CdO)x (ZnO)1-x NPs. The phase analysis using EDX spectroscopy and FTIR spectroscopy confirmed the presence of Cd and Zn as the original compounds of prepared (CdO)x (ZnO)1-x NP samples. The average particle size of the samples increased from 14 to 33 nm as the concentration of precursor increased from x=0.20 to x=0.80, as observed by TEM results. The surface composition and valance state of the prepared product NPs were determined by X-ray photoelectron spectroscopy (XPS) analyses. Diffuse UV-visible reflectance spectra were used to determine the optical band gap through the Kubelka-Munk equation; the energy band gap was found to decrease for CdO from 2.92 to 2.82 eV and for ZnO from 3.22 to 3.11 eV with increasing x value. Additionally, photoluminescence (PL) spectra revealed that the intensity in PL increased with an increase in particle size. In addition, the antibacterial activity of binary oxide NP was carried out in vitro against Escherichia coli ATCC 25922 Gram (-ve), Salmonella choleraesuis ATCC 10708, and Bacillus subtilis UPMC 1175 Gram (+ve). This study indicated that the zone of inhibition of 21 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.