Structure and photocatalytic properties of copper-doped rutile TiO2 prepared by a low-temperature process

Copper-doped titania with variable Cu/Ti ratios have been prepared via a simple aqueous-phase method at 85 °C. The obtained products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and UV-vis absorption spectra analysis. The photocatalytic properties of the products were tested by photocatalytic degradation of aqueous brilliant red X-3B solution. The results showed that the sample with 2% copper doping has the best photocatalytic activity, which is 3 times that of undoped rutile titania. The effect of the doped copper on the structure and property of TiO₂ has also been discussed.     

Elaboration and characterization of TiO2 nanoparticles incorporated in SiO2 host matrix

Nanometer-scale TiO₂ particles have been synthesized by sol-gel method. It was incorporated in a glass-based silica aerogel. The composite was characterized by various techniques such as particle size analysis, scanning electron microscopy (SEM), atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray diffraction (XRD), infrared spectroscopy (IR) and photoluminescence (PL). The bulk glass presents a strong luminescence at wavelengths ranging from 750 to 950 nm. This PL was attributed to various non-bridging oxygen hole centers (NBOHCs) defects resulting from thermal treatment and crystallization of TiO₂ at the interface between titania nanoparticles and silica host matrix.     

Versatile fabrication of dendritic cobalt microstructures using CTAB in high alkali media

A facile hydrothermal reduction route based on a precipitate slow-release controlled process was developed to fabricate highly ordered dendritic cobalt microcrystals using cetyltrimethylammonium bromide (CTAB) in high alkali media. The shape, structure, and magnetic properties of the final products were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), electron diffraction (ED), and vibrating sample magnetometry (VSM). The results showed that the sample is hexagonal close-packed Co coexisting with cubic close-packed Co; the length of the main trunk is about 8 μm and diameter of the branches is 0.5-2 μm. Magnetic measurement at 300 K showed that these microstructures exhibited ferromagnetic character. The probable formation mechanism of the microcrystals was discussed on the basis of the experimental results.     

Effect of precursor preoxidation on the structure of phenolic resin-based activated carbon spheres

Activated carbon spheres with 3D hierarchical porous structure were prepared from phenol-formaldehyde resins with oxidation treatment in air and physical activation in an inert atmosphere. Based on the results of thermogravimetric analysis, infrared spectrometer (IR), scanning electron microscopy (SEM) and nitrogen adsorption/desorption, the effect of preoxidation on the morphology and structure of activated carbon spheres was investigated. The results show that decomposition and crosslinking reactions occur during the preoxidation and the structural changes of precursor generated by the preoxidation lead to differences in the pore structure of activated carbon spheres. The carbon spheres exhibit the unique 3D hierarchical porous structure, high specific surface area of 1897 m²/g and high pore volume of 2.22 cm³/g.     

Gallate-Zn-Al-layered double hydroxide as an intercalated compound with new controlled release formulation of anticarcinogenic agent

A new organic-clay material, in which the organic moiety is intercalated into the inorganic interlayer, was prepared using gallate anion (GA) as a guest, and Zn-Al-layered double hydroxide, as clay host. The ion-exchange technique was found to be effective for the intercalation process in the formation of the compound. Although the basal spacings of the LDH and its intercalated product were fairly similar, FTIR, CHNS and TGA/DTG results indicated that the GA was actually intercalated into the interlayer of the host in parallel orientation. The resulting nanostructure material possessed a well ordered layered structure with 42.2% GA loading (w/w). The release of the anion from the interlayer of the intercalated compound was found to be of controlled manner, governed by the first order kinetic and it was also concentration dependent. The material has potential as a nano-storage of anticarcenogenic agent with controlled delivery capability.     

Controlled preparation of unsupported binary and ternary sulfides with high surface area from tetraalkylammonium thiosalts

Unsupported MoS₂, WS₂ and Ni-MoS₂ sulfides have been successfully prepared by decomposition of tetraalkylammonium thiosalts, which were synthesized by using an aqueous solution of tetraalkylammonium halide and ammonium thiosalts at room temperature. The as-prepared samples were characterized by N₂ physorption, thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results showed that structures and properties of unsupported binary and ternary sulfides depended on tetraalkylammonium thiosalts and decomposition conditions. The samples formed by decomposition of methyl and cetyltrimethyl substituted ammonium thiosalts exhibited high specific surface areas of above 100 m²/g, indicating the organic ligand in the precursor can tune the structure of the binary and ternary sulfides. MoS₂ and Ni-MoS₂ prepared from TMetATM and Ni/TMetATM had a relative narrow distribution in mesoporous range. TEM and XRD results revealed that the unsupported binary and ternary sulfides consisted of few-stacked layers and Ni was well-dispersed on MoS₂.     

Two different approaches to synthesizing Mg-Al-layered double hydroxides as folic acid carriers

Layered double hydroxides (LDHs) are a class of artificially constructed materials that have potential applications in a wide range of fields, including biomedical research and drug development. In this study, we have successfully intercalated folic acid into LDH using two different approaches: co-precipitation and ion exchange. The resultant LDH-folic acid constructs were then characterized by powdered sample X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), thermogravimetry and differential thermal analysis (TG-DTA). XRD data demonstrated that folic acid molecules remained intact and stable between the hydroxide layers in LDH particles constructed by both co-precipitation and ion-exchange methods, with interlayer spacings of 15.3 and 16.0 Å, respectively. Particle size and surface topography were also determined using TEM. Cytotoxicity test revealed that neither LDH nor LDH-folic acid nanohybrids were toxic to the cell line 293T, suggesting that they can be used as a safe and noncytotoxic drug delivery system. Furthermore, the buffering effect of the intercalated LDH was evaluated. This work provides fundamental insights and technical details for utilizing biofunctional molecules that can form nanobiohybrid particles.     

Characterization, sintering and dielectric properties of nanocrystalline zinc oxide prepared by a citric acid-based combustion route

Nanosized zinc oxide has been synthesized through a novel single step solution combustion route using citric acid as fuel. The X-ray diffraction (XRD) analysis revealed that the synthesized ZnO nanopowder has the pure wurtzite structure. The phase purity of the nanopowder has been confirmed using differential thermal analysis (DTA), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FT-IR). The morphology and crystalline size of the as-prepared nanopowder characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the powder consisted of a mixture of nanoparticles and nanorods. The nanocrystalline ZnO could be sintered to ∼97% of the theoretical density at 1200 °C in 4 h. The dielectric constant (ε_r) and dielectric loss (ε_i) of sintered ZnO pellets at 5 MHz were 1.38 and 9×10⁻², respectively, at room temperature.     

t-Se microspheres with holes: Hydrothermal synthesis and growth mechanism

In the present paper, novel t-Se microspheres with holes were successfully prepared via a facile solution-phase approach at 150 °C for 20 h, employing SeO₂ and glucose as reagents, poly(vinylpyrrolidone) (PVP) as the surfactant. The phase and morphology of the product were characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The conversion from α-Se to t-Se was investigated by a series of experiments and a possible formation process was suggested based on the experimental results.     

Synthesis process of nanowired Al/CuO thermite

Al/CuO nanothermites were fabricated by thermal oxidation of copper layer at 450 °C for 5 h and by aluminum thermal evaporation: thermal evaporation allows producing thin layer less than 2 μm in size. The copper has been deposited by electroplating or thermal evaporation depending on the required thickness. The obtained diameter of Al/CuO nanowires is 150-250 nm. Al/CuO nanowires composite were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and differential thermal analysis (DTA). Two distinct exothermic reactions occurred at 515 and 667 °C and total energy release of this thermite is 10 kJ/cm³.     

Structural, optical and electrical characterization of antimony-substituted tin oxide nanoparticles

Antimony-doped tin oxide (ATO) nanostructures were prepared using chemical precipitation technique starting from SnCl₂, SbCl₃ as precursor compounds. The antimony composition was varied from 5 to 20 wt%. The lower resistance was observed at composition of Sn:95 and Sb:05, when compared with undoped and higher doping concentration of antimony. The average crystalline size of undoped and doped tin oxide was calculated from the X-ray diffraction (XRD) pattern and found to be in the range of 30-11 nm and it was further confirmed from the transmission electron microscopy (TEM) studies. The scanning electron microscopy (SEM) analysis showed that the nanoparticles agglomerates forming spherical-shaped particles of few hundreds nanometers. The samples were further analyzed by energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and electrical resistance measurements.     

Preparation,characterization and photocatalytic performance of noble metals (Ag,Pd, Pt,Rh) deposited on sponge-like ZnO microcuboids

Novel sponge-like ZnO microcuboids with a hierarchical structure were fabricated via an alcoholic thermal process. Then a series of noble metals (Ag, Pd, Pt, Rh) was loaded onto the microcuboids. The samples obtained were characterized by nitrogen physical adsorption, powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectroscopy (DRS), and X-ray photoelectron spectroscopy (XPS). The results show that the ZnO microcuboids have a high surface area and a sponge-like hierarchical structure. Activity tests for the degradation of acid orange II dye showed that the noble metals enhanced the activity of ZnO to different extents. For loading of 0.5 wt.%, the activity enhancement decreased in the order Pd>Ag>Pt>Rh. Co-loading of Pd and Ag had a detrimental effect on activity compared to single loading. The enhanced photocatalytic performance can be attributed to an increase in the rate of separation of photogenerated e^–/h⁺ pairs induced by the noble metals.     

Intercalation of sulfonated melamine formaldehyde polycondensates into a hydrocalumite LDH structure

A series of sulfonated melamine formaldehyde (SMF) polycondensates possessing different anionic charge amounts and molecular weights was synthesized and incorporated into a hydrocalumite type layered double hydroxide structure using the rehydration method. For this purpose, tricalcium aluminate was dispersed in water and hydrated in the presence of these polymers. Defined inorganic–organic hybrid materials were obtained as reaction products. All SMF polymers tested intercalated readily into the hydrocalumite structure, independent of their different molecular weights (chain lengths) and anionic charge amounts. X-ray diffraction revealed typical patterns for weakly ordered, highly polymer loaded LDH materials which was confirmed via elemental analysis and thermogravimetry. IR spectroscopy suggests that the SMF polymers are interleaved between the [Ca₂Al(OH)₆]⁺ main sheets via electrostatic interaction, and that no chemical bond between the host matrix and the guest anion is formed. The SMF polymers well ensconced within the LDH structure exhibit significantly slower thermal degradation.     

Thermochromism in (Ba,Sr)-Mn oxides

Manganese based ceramic samples with composition given by the formula MeMnO₃ (Me=Ba, Sr) were prepared by solid state reaction. The preparation conditions were varied over a wide range of temperatures and the optimum sintering temperature was obtained. These materials present a change of color at low temperature (at approximately 140 K). To find the probable reason for the change of color, the materials have been characterized by various advanced techniques like X-ray diffraction (XRD), photoluminiscence, scanning and transmission electron microscopy (SEM and TEM). Studies were made at room and at low temperature. These thermochromic materials have hexagonal perovskite-like structure.     

Sol-gel synthesis of nanocomposite crystalline HMX/AP coated by resorcinol-formaldehyde

This work aims to improve the performance of composite explosive by using the sol-gel method to mix high explosive and oxidizer in nanoscale. Nanocomposite materials of HMX and AP were prepared by using resorcinol-formaldehyde (RF) as binder. Its structure was characterized by scanning electron microscopy (SEM), BET method, X-ray powder diffraction (XRD), and DSC. SEM images indicate that HMX/AP/RF aerogel has a laminate-like structure with uniform pores. The XRD results show that the mean crystal size of HMX is less than 100 nm; HMX and AP are mixed uniformly in nanoscale. The specific surface area of HMX/AP/RF is 27 m²/g and much less than that of RF aerogel. The mesopores and micropores of HMX/AP/RF aerogel mainly focus in the range of 2-20 and 0.6-1.6 nm, respectively. DSC analysis indicates that the thermal decomposition temperature of HMX/AP/RF is reduced compared to that of original HMX.     

Green synthesis of ZnO nanoparticles in a room-temperature ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide

Nanoparticles of ZnO with the wurtzite structure have been successfully synthesized via a microwave through the decomposition of zinc acetate dihydrate in an ionic liquid, 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, as a solvent. Fundamental characterizations including X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were conducted for the ZnO nanostructures.To explore the growth mechanism, the samples have been prepared in different irradiation time and also cetyltrimethylammonium bromide (CTAB) has been used as the capping reagent.     

Synthesis of In-doped Ga2O3 zigzag-shaped nanowires and optical properties

In-doped Ga₂O₃ zigzag-shaped nanowires and undoped Ga₂O₃ nanowires have been synthesized on Si substrate by thermal evaporation of mixed powders of Ga, In₂O₃ and graphite at 1000 °C without using any catalyst via a vapor-solid growth mechanism. The morphologies and microstructures of the products were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) and photoluminescence spectroscopy (PL). The nanowires range from 100 nm to several hundreds of nanometers in diameter and several tens of micrometers in length. A broad emission band from 400 to 700 nm is obtained in the PL spectrum of these nanowires at room temperature. There are two blue-emission peaks centering at 450 and 500 nm, which originate from the oxygen vacancies, gallium vacancies and gallium-oxygen vacancy pairs.     

Preparation, conversion, and comparison of the photocatalytic property of Cd(OH)2, CdO, CdS and CdSe

In this paper, we report the hydrothermal preparation of Cd(OH)₂ nanowires and further conversion to CdO nanobelts, CdS nanowires and CdSe nanoparticles through thermal treatment, solvothermal and mixed-solvothermal routes, respectively. The as-obtained products were characterized by means of powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FEMSEM). Research showed that four cadmium compounds were good photocatalysts for the degradation of organic dyes such as Safranine T and Pyronine B, under irradiation of 365 nm UV light. The order of catalytic activity of different materials was found to be Cd(OH)₂<CdO<CdS<CdSe.     

Preparation and characterization of SrSnO3 nanorods

Perovskite strontium stannate (SrSnO₃) nanorods were prepared by annealing the precursor SnSr(OH)₆ nanorods at 600 °C for 3 h. The precursor nanorods were hydrothermally synthesized at 160 °C for 16 h using Sr(NO₃)₂ and SnCl₄·5H₂O as starting materials in the presence of surfactant cetyltrimethyl ammonium bromide (CTAB). As-prepared samples were characterized by X-ray diffraction (XRD), thermogravimetric-differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and infrared ray spectroscopy (IR). The results show that the as-synthesized powders are made of SrSnO₃ one-dimensional nanorods of about 0.2-1 μm length and 100-150 nm diameter. Possible formation mechanism of SrSnO₃ with nanorod structure under certain conditions was preliminarily analyzed, in which it was thought that CTAB played an important role in the formation process of the nanorod structure. Electrochemical performance of the samples versus Li metal was also evaluated for possible use in lithium-ion batteries.     

Nanofibers and nanoplatelets of MoO3 via an electrospinning technique

Polyvinyl alcohol (PVA)/ammonium molybdate composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibers at 500 °C, MoO₃ nanofibers with a diameter of 100-150 nm were successfully obtained. MoO₃ nanoplatelets and submicron platelets were prepared by further calcinations of the MoO₃ nanofibers at 600 and 700 °C. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). A possible growth mechanism for the MoO₃ nanofibers and nanoplatelets was suggested.