Preparation of titania covered multi-walled carbon nanotube thin films

The aim of this work was to investigate the effects of relative humidity on the formation of titania layers on the surface of multi-walled carbon nanotubes under regulated conditions in a sealed system. Reactive precursor compounds such as titanium (IV) oxychloride hydrochloric acid and titanium (IV) bromide were used as precursor to cover the surface of multi-walled carbon nanotubes (MWCNTs) under solvent conditions. The mixtures of MWCNTs and titania compounds were not stirred or sonicated. The effect of relative humidity was influenced using the mixture of sulphuric acid and water in desiccators. As-prepared titan-dioxide (TiO₂) layers were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), thermogravimetric analysis (TG), X-ray diffraction (XRD) and Raman spectroscopy. Our results revealed that TiO₂ layers with different thicknesses can be obtained using this simple sealed system. These TiO₂ covered multi-walled carbon nanotube films can be ideal candidates for different kinds of applications (e.g. sensors, virus filtration or catalysts).     

The multi-staged formation process of titanium oxide nanotubes and its thermal stability

The multi-staged formation process of titanium oxide nanotubes was investigated in detail under a hydrothermal treatment. During the synthesis procedure, an intermediate stage (tree-like structures) was observed before the formation of the titanium oxide layered structures. The layered structure of titanium oxide generally was considered to exfoliate directly from raw TiO₂ materials through the alkaline hydrothermal treatment. The rolling process of the layered structures of titanium oxide was confirmed by TEM observation after the alkaline hydrothermal treatment for the raw TiO₂ materials, followed by washing with 4 M HNO₃ aqueous solution. The thermal stability of the tube products was investigated by X-ray diffraction (XRD) and scanning electron microscope (SEM). The result showed that both the morphology and crystal phase of titanium oxide nanotubes could be retained even after calcination at 650 °C.     

Low temperature facile synthesis of anatase TiO2 coated multiwalled carbon nanotube nanocomposites

Anatase TiO₂ coated multiwalled carbon nanotube (MWNT) nanocomposites were prepared by combining the sol-gel method with a self assembly technique at a low temperature. XRD, TEM, FTIR and XPS spectra were applied to characterize the crystal phase, microstructure, and other physicochemical properties of the sample. The results showed that MWNTs were covered with a 12-20 nm thickness layer of anatase TiO₂ or surrounded by a 30 -290 nm thickness coating of anatase TiO₂. The layer or coating is constructed of TiO₂ nanoparticles about 5.8 nm. Furthermore, as-prepared composite was rich in surface hydroxyl groups.     

Preparation of strain-included rutile titanium oxide thin films and influence of the strain upon optical properties

Rutile type titanium dioxide (TiO₂) thin films are prepared by pulse laser deposition (PLD) with controlled oxygen pressure. Transmission electron microscopy (TEM) analysis clarified that crystalline structures, surface structures and electric states of the TiO₂ films almost correspond to those of the bulk rutile. We observed crystalline domain including strain in the PLD film. The strain of the TiO₂ film was measured by nano-beam diffraction. The strain-included domains affected properties of the film as optical absorption. The obtained optical band gap energy value was 3.30 eV, which was larger than that of bulk. TEM results such as crystalline grain sizes and distribution were used to consider quantum size effect in order to explain the larger band gap value. Moreover the influence of strain in rutile crystalline grains upon optical properties was suggested in the present study. The difference of band gap energy between experimental and theoretically calculated ones was considered to come from the strain effects.     

Activated carbons containing TiO2: Characterization and influence of a preparation method on the state of TiO2 supported

In this study preparation procedure and characterization of coal-based activated carbons supporting TiO₂ is presented. Decomposition of titanium organic complex introduced into three raw coals of a different composition is described and illustrated by XRD patterns taken at different stages of the preparations. Influence of a coal rank and titanium supported on coals on the development of a mesoporous structure is shown. Titanium revealed a positive influence on the formation of mesopores in activated carbons. Titanium contents were higher in those carbons activated for a longer time. Loss of some part of Ti supported was observed during preparation and the loss remained in a straight relation with the activation time. As confirmed by TEM, size of TiO₂ particles supported on the activated carbons increased with the activation time. Distribution of the particles was irregular. Rutile was the only crystalline form of TiO₂ found in Ti-loaded activated carbons.     

Synthesis and characterization of anodized titanium-oxide nanotube arrays

Anodized titanium-oxide containing highly ordered, vertically oriented TiO₂ nanotube arrays is a nanomaterial architecture that shows promise for diverse applications. In this paper, an anodization synthesis using HF-free aqueous solution is described. The anodized TiO₂ film samples (amorphous, anatase, and rutile) on titanium foils were characterized with scanning electron microscopy, X-ray diffraction, and Raman spectroscopy. Additional characterization in terms of photocurrent generated by an anode consisting of a titanium foil coated by TiO₂ nanotubes was performed using an electrochemical cell. A platinum cathode was used in the electrochemical cell. Results were analyzed in terms of the efficiency of the current generated, defined as the ratio of the difference between the electrical energy output and the electrical energy input divided by the input radiation energy, with the goal of determining which phase of TiO₂ nanotubes leads to more efficient hydrogen production. It was determined that the anatase crystalline structure converts light into current more efficiently and is therefore a better photocatalytic material for hydrogen production via photoelectrochemical splitting of water.     

Bioactivity of zirconia nanotube arrays fabricated by electrochemical anodization

Zirconia nanotubes with a diameter of 50 nm and a length of 20 μm were fabricated by anodic oxidation of zirconium in (NH₄)₂SO₄ electrolyte containing NH₄F. The structure and phase composition of the zirconia nanotube layers were characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD). The bioactivity was assessed by investigating the formation of apatite on the surface of zirconia nanotubes after soaking in simulated body fluids (SBF) for 20–30 days. The results indicate that bone-like apatite can be formed on the surface of the zirconia nanotube layers in our SBF immersion experiments. Microstructure of zirconia nanotubes with apatite layer was observed by SEM. Substance and phase compositions were characterized respectively by energy dispersive X-ray spectrometer (EDS) and XRD. Our results show that zirconia nanotube layers fabricated by electrochemical anodization exhibit favorable bioactivity.     

Silicon-substituted hydroxyapatite composite coating by using vacuum-plasma spraying and its interaction with human serum albumin

The incorporation of silicon can improve the bioactivity of hydroxyapatite (HA). Silicon-substituted HA (Ca₁₀(PO₄)_6−x (SiO₄) _x (OH)_2−x , Si-HA) composite coatings on a bioactive titanium substrate were prepared by using a vacuum-plasma spraying method. The surface structure was characterized by using XRD, SEM, XRF, EDS and FTIR. The bond strength of the coating was investigated and XRD patterns showed that Ti/Si-HA coatings were similar to patterns seen for HA. The only different XRD pattern was a slight trend toward a smaller angle direction with an increase in the molar ratio of silicon. FTIR spectra showed that the most notable effect of silicon substitution was that –OH group decreased as the silicon content increased. XRD and EDS elemental analysis indicated that the content of silicon in the coating was consistent with the silicon-substituted hydroxyapatite used in spraying. A bioactive TiO₂ coating was formed on an etched surface of Ti, and the etching might improve the bond strength of the coatings. The interaction of the Ti/Si-HA coating with human serum albumin (HSA) was much greater than that of the Ti/HA coating. This might suggest that the incorporation of silicon in HA can lead to significant improvements in the bioactive performance of HA.     

The fabrication of the antibacterial paste based on TiO2 nanotubes and Ag nanoparticles-loaded TiO2 nanotubes powders

ABSTRACT

We successfully synthesised TiO₂ nanotubes (TNTs) and silver nanoparticles (Ag NPs)-loaded TiO₂ nanotubes paste. These were coated on a glass substrate by spin coating method, and their antibacterial activities were surveyed. The morphology of materials was defined by transmission electron microscopy (TEM) image; the crystalline structure and the composition of the materials were determined by X-ray diffraction (XRD) pattern and X-ray photoelectron spectroscopy (XPS). Vibrational properties of the molecules existing in the sample were investigated by Fourier transform infrared (FTIR) spectroscopy, and the transmittances of films were determined by UV–Vis transmittance spectroscopy. This research shows that the structure and morphology of TNTs did not change after they underwent the processes of paste preparing and film coating on a glass substrate. Furthermore, the transmittance of TNTs film (about 75%) is higher than Ag NPs-loaded TiO₂ nanotubes (Ag/TNTs) film (about 65%) in the visible region. Moreover, the antibacterial property of Ag/TNTs film shows its effectiveness against Escherichia coli bacteria, and the antibacterial efficiency is 99.06% for 24 h-incubation period in the dark condition.     

Effect of TiO2 nanotube length and lateral tubular spacing on photovoltaic properties of back illuminated dye sensitized solar cell

The main objective of this study is to show the effect of TiO₂ nanotube length, diameter and intertubular lateral spacings on the performance of back illuminated dye sensitized solar cells (DSSCs). The present study shows that processing short TiO₂ nanotubes with good lateral spacings could significantly improve the performance of back illuminated DSSCs. Vertically aligned, uniform sized diameter TiO₂ nanotube arrays of different tube lengths have been fabricated on Ti plates by a controlled anodization technique at different times of 24, 36, 48 and 72?h using ethylene glycol and ammonium fluoride as an electrolyte medium. Scanning electron microscopy (SEM) showed formation of nanotube arrays spread uniformly over a large area. X-ray diffraction (XRD) of TiO₂ nanotube layer revealed the presence of crystalline anatase phases. By employing the TiO₂ nanotube array anodized at 24?h showing a diameter ??80?nm and length ??1·5???m as the photo-anode for back illuminated DSSCs, a full-sun conversion efficiency (??) of 3·5 % was achieved, the highest value reported for this length of nanotubes.     

Synthesis and characterization of anatase TiO2 nanotubes and their use in dye-sensitized solar cells

Anatase TiO₂ nanotubes (NTs) with the diameter of about 12 nm and the length of several hundreds nanometers were synthesized by hydrothermal method. The samples were characterized by X-ray diffraction (XRD), transmitting electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and Brunauer–Emmet–Teller (BET) measurements. The NTs are used to make composites photoanode with pristine TiO₂ nanoparticles in dye-sensitized solar cells (DSSCs). It was found that the NT/nanoparticle ratio had a pronounced impact on the performance of solar cells. The electrode composite has better photoelectric properties than the full nanoparticle and NTs solar cells. The optimum content NTs, was found to be 5%, at which content the incident photon to current efficiency was about 63.1%, an 13.8% increment compared to that using full P25 under the same condition.     

Synthesis and characterization of metal oxide nanorod brushes

Nanorod brushes of α-Al₂O₃, MoO₃ and ZnO have been synthesized using amorphous carbon nanotube (a-CNT) brushes as the starting material. The brushes of α-Al₂O₃ and MoO₃ are made up of single crystalline nanorods. In the case of ZnO brushes, the nanorod bristles are made by the fusion of 15–25 nm size nanoparticles and are porous in nature. Metal oxide nanorod brushes thus obtained have been characterized by XRD, FESEM, TEM and Raman spectroscopy. Single crystalline ruby nanorods were obtained by introducing chromium ions during the synthesis of alumina rods.     

Synthesis and characterization of copper ions surface-doped titanium dioxide nanotubes

Copper ions surface-doped titanium dioxide nanotubes were prepared via an assembly process based on the reactions between Cu(NH₂CH₂CH₂NH₂)₂(OH)₂ and hydroxide radicals on the surface of TiO₂ nanotubes, followed by the heat treatment in air at 723 K. The as-prepared samples were characterized with infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, and fluorescence spectroscopy (FL). The photocatalytic activity of the copper ions surface-doped titanium dioxide nanotubes was investigated by photodegradation of Rhodamine B. The results showed that copper ions were successfully introduced onto the surface of TiO₂ nanotubes. And two kinds of copper species of Cu(I) and Cu(II) were found on TiO₂ surface. Copper ions act as electron trappers facilitating the separation of electrons and holes on the surface of TiO₂ nanotubes, which allows more efficiency for the photodegradation of Rhodamine B.     

Synthesis and characterization of anatase and rutile TiO2 nanorods by template-assisted method

Well-aligned anatase and rutile TiO₂ nanorods and nanotubes with a diameter of about 80–130 nm have successfully been fabricated via sol-gel template method. The prepared samples were characterized by using thermogravimetric (TG) and differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDS). The XRD results indicated that the TiO₂ nanorods were crystallized in the anatase and rutile phases, after annealing at 400–800 °C for different periods of time from 0.2 to 10 h.     

Photochemical synthesis and characterization of Ag/TiO2 nanotube composites

TiO₂ nanotubes were fabricated by a hydrothermal method. Silver nanoparticles with diameters around 3–5 nm were loaded onto the surface of TiO₂ nanotubes via a deposition approach followed by a photochemical reduction process under ultraviolet irradiation. Transmission electron microscopy (TEM), N₂ adsorption measurements, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis diffuse reflectance spectroscopy (UV-vis), and fluorescence spectroscopy (FL) were applied to characterize the as-prepared Ag/TiO₂ nanotube composites. The photocatalytic activity of the as-prepared materials was investigated by photodegrading of methyl orange. The results showed that silver particles were in zero oxidation state and highly dispersed on the surface of TiO₂ nanotubes when the concentration of Ag⁺ was low. The presence of metallic silver can help the electron-hole separation by attracting photoelectrons. The Ag/TiO₂ nanotube composites with a suitable amount of silver showed a further improvement on the photocatalytic activity for degradation of methyl orange in water.     

Sonochemical preparation of TiO2 nanoparticles in the ionic liquid 1-(3-hydroxypropyl)-3-methylimidazolium-bis(trifluoromethylsulfonyl)amide

Spherical shaped anatase nanoparticles (ø 5 nm) have been synthesized in the ionic liquid 1-(3-hydroxypropyl)-3-methylimidazolium-bis(trifluoromethanesulfonyl)amide from titanium tetraisopropoxide by ultrasound assisted synthesis under ambient conditions. XRD, EDX, TEM, XPS, Raman, UV–vis, PL and BET measurements have been employed for characterization of the nanostructure of as-prepared TiO₂. XRD and Raman measurements both show that the obtained material is crystalline with anatase structure. The morphology of TiO₂ nanoparticles was characterized by transmission electron microscopy (TEM). The bandgap of the TiO₂ nanocrystals estimated from XRD and UV–vis measurements is about 3.3 eV. The surface area of a typical sample is 177 m² g⁻¹. The synthesized anatase nanocrystals show good photocatalytic activity in the degradation of methylorange.     

Effect of titanium and titania on chemical characteristics of hydroxyapatite plasma-sprayed into water

HA and its composite particles (HA/Ti, HA/TiO₂) were plasma-sprayed into water as well as on the Ti substrate, respectively. The microstructure and phase compositions of the sprayed HA and its composite particles before and after impinging on the substrate were studied by using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The results showed that the HA in the composite particles sprayed into water had a higher crystallinity than that in the composite coating. The addition of Ti or TiO₂ could both influence the decomposition of HA, but no chemical reacting product between them was formed before and after impinging on the substrate. However, EDS analyses showed the occurrence of interdiffusion of elements between HA and TiO₂, which was favorable to enhance the cohesive strength of particles in the composite coating. The post heat treatment at 650 °C for 2 h can effectively improve the crystallinity of coating by transforming amorphous phases into HA.     

Synthesis and characterization of P-doped TiO2 nanotubes

Titanium dioxide (TiO₂) doped with phosphorus (P) was synthesized by anodization of Ti in the mixed acid electrolyte of H₃PO₄ and HF and characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and UV–vis spectrum. The morphology greatly depends on the applied voltage. The as-formed nanotubes under the optimized condition, at 20 V for 2 h, are highly ordered with ~ 200 nm in length and the average tube diameter is about 100 nm. By annealing the initial samples at different temperatures, the importance of the crystalline nature is confirmed. Significantly, the peak positions of anatase in XRD patterns shifts to lower diffraction angles with an increase in the amount of H₃PO₄ ion. A remarkable red shift of the absorption edge has been observed for the sample formed in the electrolyte of HF and H₃PO₄, which is related to the introduction of P⁵⁺ into TiO₂ crystallization and the possible impurity energy level formed in the TiO₂ band gap. The presence of P 2p state in XPS spectrum can further confirm the P⁵⁺ which can replace a part of Ti⁴⁺ has been introduced into TiO₂ crystallization. The present convenient synthesis technique can be considered to the composition of other doped oxide materials.     

Influence of calcination parameters on the TiO2 photocatalytic properties

Nanocrystalline titanium dioxide (TiO₂) powders with different crystal phase composition were obtained by controlled hydrolysis and post-thermal treatments. The physicochemical properties of the powders were investigated by XRD, TEM/EDS, N₂ physic adsorption and DRS. The results obtained show that the particle size and crystalline structure are parameters strongly dependent on the calcination conditions, mainly temperature and heating rate. The influence of the TiO₂ phase composition on its photocatalytic activity, concerning the methylene blue photodegradation was studied. It was found that higher TiO₂ photocatalytic activity is related with the co-existence of the three TiO₂ polymorphs: anatase, brookite and rutile.     

Electrospun titanium dioxide nanofibers containing hydroxyapatite and silver nanoparticles as future implant materials

In this study, a good combination consisting of electrospun titanium dioxide (TiO₂) nanofibers incorporated with high purity hydroxyapatite (HAp) nanoparticles (NPs) and antimicrobial silver NPs is introduced for hard tissue engineering applications. The synthesized nanofibers were characterized by various state of art techniques like; SEM, XRD, TEM, TEM EDS and XPS analyses. SEM results confirmed well oriented nanofibers and good dispersion of HAp and silver NPs, respectively. XRD results demonstrated well crystalline feature of three components used for electrospinning. Silver NPs were having a diameter in range of 5–8 nm indicated by TEM analysis. Moreover, TEM EDS analysis demonstrated the presence of each component with good dispersion over TiO₂ nanofiber. The surface analyses of nanofibers were investigated by XPS which indicated the presence of silver NPs on the surfaces of nanofibers. The obtained nanofibers were checked for antimicrobial activity by using two model organisms E. coli and S. aureus. Subsequently, antimicrobial tests have indicated that the prepared nanofibers do posses high bactericidal effect. Accordingly, these results strongly recommend the use of obtained nanofiber mats as future implant materials.