Improved photodegradation activity of TiO2 via decoration with SnS2 nanoparticles

The particles of TiO₂ modified with various amounts of SnS₂ nanoparticles (TiO₂/SnS₂) were synthesized via the hydrothermal method by reacting SnCl₄·5H₂O with thioacetamide in 5% (vol.) acetic acid aqueous solution in the presence of TiO₂. The obtained products were characterized by using X-ray diffraction, X-ray photoelectron spectroscopy, UV–Vis diffuse reflection spectra, scanning and transmission electron microscopy. The photodegradation activities of TiO₂/SnS₂ composites have been investigated by using methyl orange as target in water under the light irradiation of 250–400, 360–600 and 400–600 nm. It was found that the photodegradation activity of TiO₂/SnS₂ composites depended on the mass ratio of SnS₂ and the wavelength of the irradiating light. The composites containing 33% SnS₂ exhibited the maximum activity under the light irradiation of 250–400 and 360–600 nm. However, the more SnS₂ in the composites, the higher activity appeared under the irradiation of 400–600 nm light. All the results reveal that the composites possess much better activity than the pristine TiO_2.     

Structural,spectroscopic and biological investigation of copper oxides nanoparticles with various capping agents

Powder composed of copper oxides nanoparticles with various capping agents has been synthesized and characterized with the use of X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Polyvinyl alcohol (PVA), glycol propylene, glycerin and glycerin plus ammonia were used as capping agents. The scanning electron microscopy (SEM) studies showed that nanoparticles form agglomerates with the size from 80 to 120 nm while particles size determined from the XRD experiment was in the range from 7 to 21 nm. XPS and XRD experiments revealed that depending on capping and reducing agents used in the synthesis nanoparticles are composed of Cu₂O, CuO or a mixture of them. The biological activity test performed for a selected sample where the capping agent was glycerin plus ammonia has shown promising killing/inhibiting behavior, very effective especially for Gram negatives bacteria.     

Real time X-ray scattering study of the formation of ZnS nanoparticles using synchrotron radiation

We investigate the growth of ZnS nanoparticles by a real-time simultaneous small and wide angle X-ray scattering (SAXS, WAXS) study using synchrotron radiation. Zinc chloride and elemental sulfur were dissolved in oleylamine. The formation of nanoparticles was induced by heating to 170 °C and 215 °C. The influence of temperature, reaction time, and sulfur concentration was investigated. After a short phase of rapid growth, saturation in size and a slower growth is observed depending on the temperature. The final size of the nanoparticles ranges between 2 and 6 nm for the investigated growth conditions and increases with the reaction temperature and sulfur concentration. SAXS analysis allows for determination of the size of the nanoparticles and proves also the existence of an organized layer of oleylamine molecules covering the nanoparticles' surfaces, which, however, appears only for diameters of the nanoparticles larger than approximately 2.8 nm. The investigation of the measured structure factor of the nanoparticle assemblies showed that the distance of an attractive interaction is 2.5 nm, which was interpreted as a consequence of the ordered oleylamine surface layer.     

The effect of Pt nanoparticles loading on H2 sensing properties of flame-spray-made SnO2 sensing films

SnO₂ nanoparticles loaded with 0.2–2 wt% Pt have successfully been synthesized in a single step by flame spray pyrolysis (FSP) and investigated for gas sensing towards hydrogen (H₂). According to characterization results by X-ray diffraction, nitrogen adsorption, scanning/high resolution-transmission electron microscopy and analyses based on Hume-Rothery rules using atomic radii, crystal structure, electronegativities, and valency/oxidation states of Pt and Sn, it is conclusive that Pt is not solute in SnO₂ crystal but forms nanoparticles loaded on SnO₂ surface. H₂ gas sensing was studied at 200–10,000 ppm and 150–350 °C in dry air. It was found that H₂ response was enhanced by more than one order of magnitude with a small Pt loading concentration of 0.2 wt% but further increase of Pt loading amount resulted in deteriorated H₂-sensing performance. The optimal SnO₂ sensing film (0.2 wt% Pt-loaded SnO₂, 20 μm in thickness) showed an optimum H₂ response of ∼150.2 at 10,000 ppm and very short response time in a few seconds at a low optimal operating temperature of 200 °C. In addition, the response tended to increase linearly and the response times decreased drastically with increasing H₂ concentration. Moreover, the selectivity against carbon monoxide (CO) and acetylene (C₂H₂) gases was also found to be considerably improved with the small amount of Pt loading. The H₂ response dependence on Pt concentration can be explained based on the spillover mechanism, which is highly effective only when Pt catalyst is well-dispersed at the low Pt loading concentration of 0.2 wt%.     

Influence of stirring in the synthesis of gold nanorods

Gold nanorods have been prepared by the seed-mediated growth method, in order to find the effect of stirring during the synthesis to the final shape and optical properties. The presence or absence of stirring during each step of the preparation procedure was considered a parameter to control in order to adjust the optical absorption associated with the surface plasmon resonance of the nanorods. Results show that the longitudinal surface plasmon resonance band shifts to larger wavelengths in the absence of stirring of the growth solution. Width and intensity of the absorption band associated with the longitudinal surface plasmon is reduced upon stirring during the synthesis. On the contrary, the position of the transversal surface plasmon resonance band scarcely depends upon stirring. Theoretical calculations performed using the Gans model are coherent with experimental obtained results, showing that as the aspect ratio increases, longitudinal plasmons absorption shifts toward larger wavelengths and increases both intensity and bandwidth.     

Influence of Fe nanoparticles diameters on the structure and electron emission studies of carbon nanotubes and multilayer graphene

In this paper we report the effect of Fe film thickness on the growth, structure and electron emission characteristics of carbon nanotubes (CNTs) and multilayer graphene deposited on Si substrate. It is observed that the number of graphitic shells in carbon nanostructures (CNs) varies with the thickness of the catalyst depending on the average size of nanoparticles. Further, the Fe nanoparticles do not catalyze beyond a particular size of nanoclusters leading to the formation of multilayer graphene structure, instead of carbon nanotubes (CNTs). It is observed that the crystallinity of CNs enhances upon increasing the catalyst thickness. Multilayer graphene structures show improved crystallinity in comparison to CNTs as graphitic to defect mode intensity ratio (I_D/I_G) decreases from 1.2 to 0.8. However, I_2D/I_G value for multilayer graphene is found to be 1.1 confirming the presence of at least 10 layers of graphene in these samples. CNTs with smaller diameter show better electron emission properties with enhancement factor (γ_C = 2.8 × 10³) in comparison to multilayer graphene structure (γ_C = 1.5 × 10³). The better emission characteristics in CNTs are explained due to combination of electrons from edges as well as centers in comparison to the multilayer graphene.     

Magnetic and dielectric properties of HoMnO3 nanoparticles synthesized by the polymerized complex method

In this paper, we report on the magnetic and dielectric properties of HoMnO₃ nanoparticles with different size synthesized by a polymerized complex method have been investigated. The HoMnO₃ nanoparticles crystallized in hexagonal perovskite-type structure. The zero-field-cooled magnetic susceptibility curve of HoMnO₃ nanoparticles with averaged size of 30 nm shows that complicated magnetic transitions occurred in a temperature range from 2 to 100 K, which was confirmed by magnetic hysteresis loops. With increasing the particle size, the antiferromagnetic (AFM) transition temperature increases from 56 to 77 K, due to the reduced surface-to-volume ratio. Moreover, with a decrease in particle size, the Mn-spin reorientation temperature (T_SR) is enhanced from 44 to 48 K.     

X-ray photoelectron spectroscopy (XPS) and FTIR studies of vanadium barium phosphate glasses

Barium vanadophosphate glasses, having composition 50BaO–xV₂O₅–(50 − x)P₂O₅, (x = 0–50 mol%), were prepared by conventional melt quench method. Density, molar volume and glass transition temperature (T_g) were measured as a function of V₂O₅ content. Structural investigation was done using XPS and FTIR spectroscopy. First, substitution of the P₂O₅ by the V₂O₅ in the metaphosphate 50BaO–50P₂O₅ glass increases the density and T_g and decreases the molar volume. When the amount of V₂O₅ increases, all these properties show a reverse trend. XPS measurement found in the O1s, P2p, and V2p core level spectra indicate the presence of primarily P–O–P, P–O–V and V–O–V structural bonds, the asymmetry in the P 2p spectra indeed arises from the spin-orbit splitting of P 2p core level, and more than one valence state of V ions being present. IR spectroscopy reveals the depolymerization of the phosphate glass network by systematic conversion of metaphosphate chains into pyrophosphate groups and then orthophosphate groups. Even though metaphosphate to pyrophosphate conversion is taking place due to breaking of P–O–P linkages, formation of P–O–V and P–O–Ba linkages provide cross linking between short P-structural units, which make the glass network more rigid. Above 10–20 mol% V₂O₅ content, network is highly depolymerized due to the formation of orthophosphate units and V–O–V bridge bonds, resulting in poor cross-linking, making the glass network less rigid.     

Gold and silver nanoparticles surface functionalized with rhenium carbonyl complexes

Gold and silver nanoparticles have been synthesized and stabilized with 3-mercaptopropionic acid (MPA). The resulting MPA capped nanoparticles have been functionalized by attaching rhenium carbonyl species to the MPA carboxylate groups. The whole process have been carried out in a two-step procedure improved from the literature for radiopharmaceutical applications. The resultant rhenium-coated metal (gold or silver) nanoparticles have been studied by a different techniques, as for example X-ray photoelectron spectroscopy, UV–Visible spectroscopy, Z-potential, thermogravimetric analysis and vibrational infrared spectroscopy, which proves that the metal core has been really coated with the rhenium carbonyl species, so X-ray diffraction and transmission electron microscopy have been used to study the structure, size and shape of the obtained nanoparticles.     

Facile synthesis of α-MnO2 nanorods at low temperature and their microwave absorption properties

One-dimensional α-MnO₂ nanorods were fabricated by using low-temperature water-bathing chemical precipitation method at 80 °C. The crystalline structures, morphological evolution process and microwave absorption properties were systematically investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and measurement of electromagnetic parameters. The results show that the morphological structures and electromagnetic properties have close relationship with the reaction time. With the prolonging of the treatment time, the as-synthesized products turn from microspheres constituted of tiny dendrites to nanorods with diameters of 20–30 nm and lengths up to 1–2 μm. The electromagnetic characterization shows that the dielectric constants and magnetic permeability values show decreasing trends with the increasing frequency, however, the dielectric and magnetic loss tangents all increase with frequency. The electromagnetic absorption properties of the products have close relationship with the morphologies and thicknesses of the samples. With a thickness of 3 mm, an absorbing peak value of −25 dB was achieved for the sample treated for 24 h. The microwave absorption properties of MnO₂ can be attributed mainly to interfacial polarization, space charge polarization and relaxation phenomena.     

Finestructures study of the diamond/titanium interface by transmission electron microscopy

It is well known that a TiC layer can be formed and should act as a buffer layer in diamond films deposited on Ti alloy. Through our cross-sectional investigation in HRTEM, a thin layer (20–30 nm) was first identified between the outermost diamond film and the inner reactive TiC layer adjacent to the substrate. This layer consists of numerous crystalline nanoparticles with grain sizes of 5–20 nm. Through electron nanodiffraction patterns combined with EDS and EELS analysis, these nanoparticles can be identified as a TiC_1−xO_x phase with a similar structure to cubic TiC. Besides, C atoms and O atoms in TiC_1−xO_x randomly occupy the vacancies of C in TiC. The thickness of this TiC_1−xO_x layer does not change significantly with increasing deposition time, and the diamond phase directly nucleates and grows on it.     

Faceted MoS2 nanotubes and nanoflowers

A simple synthesis of novel faceted MoS₂ nanotubes (NTs) and nanoflowers (NFs) starting from molybdenum oxide and thiourea as the sulphur source is reported. The MoS₂ nanotubes with the faceted morphology have not been observed before. Further the as-synthesized MoS₂ nanotubes have high internal surface area. The nanostructures have been characterized by a variety of electron microscopy techniques. It is expected that these MoS₂ nanostrutures will find important applications in energy storage, catalysis and field emission.     

Microtexture and structure of boron nitride fibres by transmission electron microscopy, X-ray diffraction, photoelectron spectroscopy and Raman scattering

Continuous boron nitride fibres have been fabricated by melt spinning and pyrolysis of poly[2,4,6-tris(methylamino)borazine]. The longitudinal mechanical properties depend on mechanical stress and temperature applied during the conversion process. High-performance and low-performance fibres were characterized in order to find relationship between structure and physical properties. In all the cases, photoelectron spectroscopy (XPS) analysis proves that the chemical composition of the fibre is close to stoichiometric BN. The crystallite sizes were measured by means of X-ray diffraction (XRD) and Raman techniques. Cross-sections of separated fibres were investigated by high-resolution electron microscopy (HREM) and transmission electron microscopy (TEM). All the BN fibres have a hexagonal turbostratic structure. With increasing stress and temperature, the tensile strength and the elastic modulus increase. In the high-performance fibres, the 002 layers with an increased distance (about 0.35 nm) showed a mean stacking sequence near to graphite and a preferred orientation of the 002 layers parallel to the fibre axis.     

The role of Ag particles deposited on TiO2 or Al2O3 self-organized nanoporous layers in their behavior as SERS-active and biomedical substrates

In this paper, we present recent results of investigations of hybrid materials consisting of nanoporous oxides layers loaded with Ag nanoparticles: Ag/TiO₂-n/Ti and Ag/Al₂O₃-n/Al (where “n-“stands for nanotubes), which could be used as active SERS substrates or as bioactive materials in medicine (implants). Simple electrochemical, chemical and physical methods appear suitable for fabricating such hybrid materials having different functional properties.     

Ultrasonic spray pyrolysis of surface modified TiO2 nanoparticles with dopamine

Spherical, submicronic TiO₂ powder particles were prepared in the low temperature process of ultrasonic spray pyrolysis (150 °C) by using as a precursor aqueous colloidal solutions consisting of surface modified 45 Å TiO₂ nanoparticles with dopamine. Detailed structural and morphological characterization of colored submicronic TiO₂ spheres was performed by X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), laser particle size analysis and FTIR techniques. Also, optical characterization of both dopamine-modified TiO₂ precursor nanoparticles and submicronic TiO₂ powder particles was performed using absorption and diffuse reflectance spectroscopy, respectively. A significant decrease of the effective band gap (1.9 eV) in dopamine-modified TiO₂ nanoparticles compared to the band gap of bulk material (3.2 eV) was preserved after formation of submicronic TiO₂ powder particles in the process of ultrasonic spray pyrolysis under mild experimental conditions. Due to the nanostructured nature, surface-modified assemblage of TiO₂ nanoparticles preserved unique ability to absorb light through charge transfer complex by photoexcitation of the ligand-to-TiO₂ band, conventionally associated with extremely small TiO₂ nanoparticles (d < 20 nm) whose surface Ti atoms, owing to the large curvature, have penta-coordinate geometry.     

Scanning transmission electron microscopy (STEM)-transmission electron microscopy (TEM) analysis of nitrogen ion implanted austenitic 302 stainless steel

The microstructure of nitrogen implanted AISI 302 austenitic stainless steel and the effect of long-term room temperature ageing on it have been studied. Samples were implanted in 1992 with 2.5×10²¹ N₂⁺ m⁻² at 130 keV. The characteristics of the implanted layer and the depth profile have been investigated by scanning transmission electron microscope combined with energy dispersive X-ray spectrometry. Electron diffraction patterns recorded in the implanted layer using transmission electron microscopy confirm the formation of CrN along with the presence of Cr₂N. The identification of phases by glancing angle X-ray diffraction also indicates the formation of Cr₂N and nitrogen solid solutions. The effects of ageing on the microstructure are observed to be small.     

Sonochemical synthesis,characterization, and electrochemical properties of MnMoO4 nanorods for supercapacitor applications

In this article, we reported the preparation of manganese molybdate (MnMoO₄) nanorods by a facile sonochemical method and investigated its electrochemical properties for supercapacitor applications. The microstructure, surface morphology and composition were characterized by using field emission scanning electron microscope (FE-SEM), high resolution-transmission electron microscopy (HR-TEM), X-ray diffraction analysis (XRD), Raman spectroscopy and X-ray photo electron microscopy (XPS). The cyclic voltammetry (CV) curves of sonochemically synthesized α-MnMoO₄ nanorods revealed the presence of redox pairs suggesting the pseudocapacitive nature of MnMoO₄. A maximum specific capacitance of the α-MnMoO₄ nanorods was about 168.32 F g⁻¹ as observed from the galvanostatic charge–discharge (GCD) analysis at a constant current density of 0.5 mA cm⁻². Long term cyclic stability study revealed that about 96% of initial capacitance was retained after 2000 cycles.     

Synthesis of Fe-Ti-MCM-48 from silatrane precursor via sol-gel process and its hydrothermal stability

A series of bimetallic Fe–Ti-MCM-48 materials was successfully synthesized via sol–gel method using cetyltrimethylammonium bromide (CTAB) as a template and silatrane, iron (III) chloride, and titanium (IV) isopropoxide as silica, iron, and titanium sources, respectively. Scanning electron microscopy (SEM) showed the truncated octahedron morphology of Fe–Ti-MCM-48.X-ray diffraction (XRD) patterns showed well-defined, order cubic mesoporous structures. X-ray fluorescence (XRF) revealed the total metal content of the final product. UV–visible absorption spectra confirmed both iron (Fe³⁺) and cerium (Ti⁴⁺) species highly dispersed in the framework, while N₂ adsorption/desorption measurements indicated a high specific surface area. As metal content increased, the mesoporous order and surface area decreased. The synthesized Fe–Ti-MCM-48 with 0.01Fe/Si and 0.01Ti/Si ratio still retained a cubic structure after hydrothermal treatment at 100 °C for 72 h.     

Synthesis,characterization and formaldehyde gas sensitivity of La0.7Sr0.3FeO3 nanoparticles assembled nanowires

La_0.7Sr_0.3FeO₃ nanoparticles assembled nanowires were synthesized by a hydrothermal method assisted with cetyltrimethylammonium bromide (CTAB). The hydrothermal temperature was 180 °C and the annealed temperature was 700 °C. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the morphology, composition and structural properties of the materials. The results showed that the La_0.7Sr_0.3FeO₃ nanoparticles assembled nanowires had a high aspect ratio (the largest aspect ratio >100); the size of the nanoparticles was about 20 nm and the diameter of the nanowires was about 100–150 nm. The growth mechanism of La_0.7Sr_0.3FeO₃ nanowires was discussed. Gas sensors were fabricated by using La_0.7Sr_0.3FeO₃ nanowires. Formaldehyde gas sensing properties were carried out in the concentration range of 0.1–100 ppm at the optimum operating temperature of 280 °C. The response and recovery times to 20 ppm formaldehyde of the sensor were 110 s and 50 s, respectively. The gas sensing mechanism of La_0.7Sr_0.3FeO₃ nanowires was investigated.     

Cerium incorporating into MCM-41 mesoporous materials for CO oxidation

Ceria doped MCM-41 materials were synthesized by surfactant-assisted hydrothermal and wet impregnation methods. All the obtained Ce-MCM-41 materials were characterized by N₂ physical adsorption, X-ray diffraction (XRD), diffuse reflectance UV–visible spectroscopy (DRUV–vis), infrared spectroscopy (IR), solid-state cross-polarization magic angle spinning nuclear magnetic resonance spectroscopy (CP/MAS-NMR), and transmission electron microscopy (TEM). The catalytic properties were evaluated in CO oxidation under atmospheric pressure and various temperatures. The results showed that in the materials synthesized by hydrothermal method, most of Ce ions were well incorporated in the tetrahedral coordinated sites into the framework of the MCM-41 as Si/Ce molar ratio is 30 and 50. High cerium content may lead to mesostructure partial collapsing and ceria particles segregation. For CO oxidation, the catalytic activity of Ce-MCM-41 synthesized by hydrothermal method was significantly greater than that of the materials prepared by impregnation route. Over the Ce-MCM-41 materials prepared via hydrothermal technique, 100% CO conversion was achieved at 504, 514 and 528 K, respectively, as the Si/Ce molar ratio decreased from 50 to 30 and 10. For the first time, we found an interesting correlation of Q₃ species relative area in the ²⁹Si CP/MAS-NMR spectra of the Ce-MCM-41materials with the reaction rates of CO oxidation, which indicates that both surface hydroxyls and tetrahedral-coordinated Ce⁴⁺ ions in the MCM-41 take important roles in the CO oxidation.