Fabrication of nanoporous Sr incorporated TiO2 coating on 316L SS: Evaluation of bioactivity and corrosion protection

In this paper, nanoporous TiO₂ and Sr-incorporated TiO₂ coated 316L SS were prepared by sol–gel methodology. The effect of Sr incorporation into TiO₂ coating on bioactivity and corrosion resistance was investigated. Attenuated total reflectance–Fourier transform infrared (ATR–FTIR) spectroscopy, X-ray diffraction analysis (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) results obtained after in vitro bioactivity test confirm the excellent growth of crystalline hydroxyapatite (HAp) over nanoporous Sr-incorporated TiO₂ coated 316L SS which may be attributed to the slow and steady release of Sr ions from the coatings. The electrochemical evaluation of the coatings confirms that Sr-incorporated TiO₂ coating offer excellent protection to 316L SS by acting as a barrier layer. The results showed that the incorporation of Sr enhanced both bioactivity and corrosion resistance of 316L SS. Hence Sr-incorporated TiO₂ coated 316L SS is a promising material for orthopaedic implant applications.     

Synthesis and characterization of photosensitive TiO<Subscript>2</Subscript> nanorods by controlled precipitation route

Nanocrystalline TiO₂ thin films have been successfully synthesized by controlled precipitation route. These films are further annealed at 623 K for 2 h. The change in structural, morphological, optical, and wettability properties are studied by means of X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), scanning electron microscopy (SEM), optical absorption, and contact angle measurement. From the XRD pattern it is clear that the as-grown TiO₂ films are amorphous in nature which becomes polycrystalline after annealing. The FTIR study reveals the formation of TiO₂ compound. Scanning electron micrographs shows that the as-grown TiO₂ film consists of agglomerated nanograins well covered to the substrate surface which gets converted into vertical nanorods after annealing. As-deposited and annealed TiO₂ films showed hydrophilic behavior as water contact angles were 24° and 32°, respectively. The optical absorption study reveals the small red shift due to annealing and attributed to grain size. The annealed TiO₂ film showed conversion efficiency of 0.037% in photoelectrochemical cell with 1 M NaOH electrolyte.     

Growth of hydrophobic TiO2 on wood surface using a hydrothermal method

Hydrophobic titanium dioxide (TiO₂) was successfully grown on a wood surface using a hydrothermal method. Energy dispersive X-ray spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and water contact angle (WCA) were employed to characterize the features of grown TiO₂ and its hydrophobicity. EDS, XRD, and FTIR proved that anatase TiO₂ chemically bonded to the wood surface through the combination of hydrogen groups during the hydrothermal process. The values of WCAs manifested that the hydrophobicity of the treated wood was mainly dependent on specific reaction conditions, especially on reaction pH value and hydrothermal temperature. The highest WCA reached 154° when the hydrothermal temperature was 130 °C. The treated wood thus possessed a superhydrophobic surface.     

Preparation and characterization of photocatalytic TiO<Subscript>2</Subscript> films on functionalized stainless steel

In this study, TiO₂ was synthesized using controlled hydrolysis of TiCl₄, followed by dialysis. We produced a transparent emulsion that was later dried into TiO₂ powder. TiO₂ photocatalyst films were deposited applying the technique of pulsed electrophoretic deposition, which decreased bubble formation caused by direct current. The substrates were bare stainless steel (SS) and stainless steel pre-functionalized in a conversion bath. Film surface morphology, crystallinity, elemental composition, and wettability were determined using XRD, SEM–EDAX, and contact angle measurements. The mechanical properties were determined by nano-indentation test. The adhesion was investigated using scratch test. The obtained results showed that the TiO₂ film over a conversion layer had better adhesion and mechanical properties than TiO₂ over bare SS. The optical characteristics of TiO₂ films were tested using PL measurement. The photocatalytic decolourization of the amido black-10B dye was studied over TiO₂ coating under UV and visible light irradiation. TiO₂ film over a conversion layer without heat treatment exhibited the best photocatalytic activity as a result of its crystalline size and three-phase structure as well as the synergetic effect of TiO₂ and Fe₂O₃.     

Rapid synthesis, characterization and optical properties of TiO2 coated ZnO nanocomposite particles by a novel microwave irradiation method

A novel and rapid microwave method was used to prepare TiO₂ coated ZnO nanocomposite particles. The resulted particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Results show that ZnO nanoparticles were coated with 6-10 nm amorphous TiO₂ layers. In addition, zeta potential analysis demonstrated the presence of TiO₂ layer on the surface of ZnO nanoparticles. Photoluminescence (PL) spectroscopy and UV-visible spectroscopy were used to investigate the optical properties of the nanoparticles. Compared to uncoated ZnO nanoparticles, the TiO₂ coated ZnO nanoparticles showed enhanced UV emission. The UV-visible diffuse reflectance study revealed the significant UV shielding characteristics of the nanocomposite particles. Moreover, amorphous TiO₂ coating effectively reduced the photocatalytic activity of ZnO nanoparticles as evidenced by the photodegradation of Orange G with uncoated and TiO₂ coated ZnO nanoparticles under UV radiation.     

Sol–gel derived hydroxyapatite/titania biocoatings on titanium substrate

A simple sol–gel method was successfully developed for a hydroxyapatite (HA)/TiO₂ double layer deposition on a pure titanium substrate. Phase formation, surface morphology, and interfacial microstructure were investigated by differential scanning calorimetry analysis (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The TiO₂ layer was coated by a spin coating method at a speed of 1500 rpm for 15 s, followed by a heat treatment at 560 °C for 20 min. The HA film was subsequently spin coated on the outer surface at the same speed and then heat-treated at difference temperatures. Results indicated that the HA phase began to crystallize after a heat treatment at 580 °C; and the crystallinity increased obviously at a temperature of 780 °C. The HA film showed a porous structure and a thickness of 5–7 μm after the heat treatment at 780 °C. SEM observations revealed no delamination and crack at the interfaces of HA/TiO₂ and TiO₂/Ti. The HA film with a porous structure is expected to be more susceptible to the natural remodeling processes when it is implanted in a living body.     

Synthesis and characterization of nanocrystalline TiO<Subscript>2</Subscript> thin films

Nanocrystalline thin films of TiO₂ have been synthesized by sol gel spin coating technique Thin films of TiO₂ annealed at 700 °C were characterized by X-ray diffraction(XRD), Atomic Force Microscopy, High resolution TEM and Scanning Electron Microscopy (SEM), The XRD shows formation of tetragonal anatase and rutile phases with lattice parameters a = 3.7837 Å and c = 9.5087 Å. The surface morphology of the TiO₂ films showed that the nanoparticles are fine with an average grain size of about 60 nm. Optical studies revealed a high absorption coefficient (10⁴ cm^?1) with a direct band gap of 3.24 eV. The films are of the n type conduction with room temperature electrical conductivity of 10^?6 (Ω cm)^?1.     

Growth and characterization of hydroxyapatite nanorice on TiO2 nanofibers

Hydroxyapatite (HA) coating with nanoparticles like nanorice is fabricated on chemically pretreated titanium (Ti) surface, through an electrochemical deposition approach, for biomaterial applications. The Ti surface was chemically patterned with anatase TiO₂ nanofibers. These nanofibers were prepared by in situ oxidation of Ti foils in a concentrated solution of H₂O₂ and NaOH, followed by proton exchange and calcinations. Afterward, TiO₂ nanofibers on Ti substrate were coated with HA nanoparticles like nanorice. The obtained samples were annealed at high temperature to produce inter diffusion between TiO₂ and HA layers. The resultant layers were characterized by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-ray Photoelectron Spectroscopy (XPS), X-ray Diffraction (XRD), Infrared Spectroscopy (FTIR), corrosion tests in SBF solution, and Electron Probe Micro Analysis (EPMA). It was found that only Ti from the titanium substrate diffuses into the HA coating and a good corrosion resistance in simulated body fluid was obtained.     

Synthesis of silver and sulphur codoped TiO<Subscript>2</Subscript> nanoparticles for photocatalytic degradation of methylene blue

In the present work, silver and sulphur codoped TiO₂ (Ag–S/TiO₂) photocatalysts were effectively prepared by sol–gel technique. The prepared samples were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive x-ray analysis (EDX), Fourier transform infrared (FTIR) spectroscopy, diffuse reflectance UV–Vis spectroscopy (UV-DRS) and photoluminescence (PL). The XRD patterns consisted of anatase crystalline phases and the particle size and shape of the prepared samples were observed by SEM and HR-TEM. The presence of doping ions was confirmed by EDX analysis, the decreased band-gap energy of Ag–S codoped TiO₂ nanoparticles was investigated by UV-DRS. The decreased in the intensity of Ag–S codoped TiO₂ was absorbed due to the lower separation of electron–hole pairs were confirmed by PL spectrum. The Ag–S codoped TiO₂ showed higher photocatalytic activity than pure and single-doped TiO₂ in the photodegradation of methylene blue (MB) aqueous solution under visible light irradiation. The given work was a good model to associate the considering of the synergistic effect of metal and non-metal codoped TiO₂ in the photocatalysis and photo electrochemistry.     

Synthesis and characterization of Co-doped nano-TiO<Subscript>2</Subscript> through co-precipitation method for photocatalytic activity

The aim of this work was synthesis and investigation of various properties of Co-doped titanium dioxide nanostructures. Synthesis was conducted by the co-precipitation method using cobalt nitrate and titanium isopropoxide as a precursor, followed by thermal treatment at a temperature of 500 °C. The materials were fully characterized using several techniques (X-ray diffraction XRD, SEM, FTIR, TGA/DTA, UV–Vis diffuse reflectance DRS and photoluminescence). However, dopant has no effect on XRD pattern of the host but it can influence on the various characteristics of host such as optical and electrical properties. The scanning electron microscopy was used to detect the morphology of synthesized nanoparticles which sizes changed with the altitude in the doping concentration to 6%. FTIR spectra exhibit broad peaks where anatase phases of TiO₂ demonstrate very sharp UV–Vis band gap results showed the reduction in band gap from from 3.21 eV, for undoped TiO₂, to 2.74 eV, for Co doped 6% TiO₂. The photocatalytic activity of the samples were studied based on the degradation of methyl orange as a model compound, where the results showed that Co doped 6% TiO₂ a good photocatalytic activity.     

Hydrothermal preparation and characterization of TiO2:AC composites

A new photocatalyst titania:activated carbon (TiO₂:AC) composite was prepared by impregnating anatase type TiO₂ nanoparticulates onto the activated carbon surface through a mild hydrothermal route. A varied ratio of TiO₂ to AC was considered for impregnation. As-prepared TiO₂:AC composite was characterized by various techniques such as powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), BET surface area and positron annihilation lifetime spectroscopy (PALS). Powder XRD results showed the persisting nature of anatase phase of TiO₂ deposited on the activated carbon surface. The BET, FTIR and PALS results revealed the impregnation threshold. The TiO₂ particulates were well adhered and uniformly dispersed on the carbon surface as confirmed by SEM.     

Preparation of N-methylaniline capped mesoporous TiO2 spheres by simple wet chemical method

Pure anatase mesoporous TiO₂ nanospheres were synthesized by simple wet chemical treatment and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet–visible spectroscopy (UV–vis), Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (XRD). The results revealed that the surface morphology of the TiO₂ spheres could be controlled by adjusting the concentration of N-methylaniline and that the average diameter of the TiO₂ spheres was 600 nm. FTIR results confirmed the formation of N-methylaniline capped TiO₂ nanospheres.     

Preparation of rutile (TiO<Subscript>2</Subscript>) nanostructured materials at low temperature from TiCl<Subscript>4</Subscript> aqueous solution

The synthesis of rutile (TiO₂) nanostructured materials at low temperature from TiCl₄ aqueous solution was described. TiO₂ coatings on polystyrene (PS) particles were prepared by layer-by-layer assembly technique. The samples were characterized by DTA-TG, SEM, XPS, TEM and XRD techniques. The experimental results showed that pure rutile-TiO₂ coatings with nanocrystal structure were synthesized at 100 °C. On the surface of PS particles, sphere-type TiO₂ coatings exhibited uniform shape and a narrow size distribution. The amount of TO₂ (wt%) and shell thickness of particles increased with the adding of coating layers. Hollow TiO₂ spheres were obtained by calcination at 450 °C. TiO₂/PS with 2 coating layers showed higher degradation rate. The photocatalytic activity of hollow TiO₂ spheres was higher than that of TiO₂/PS.     

Characterization and bond strength of electrolytic HA/TiO<Subscript>2</Subscript> double layers for orthopaedic applications

Insufficient bonding of juxtaposed bone to an orthopaedic/dental implant could be caused by material surface properties that do not support new bone growth. For this reason, fabrication of biomaterials surface properties, which support osteointegration, should be one of the key objectives in the design of the next generation of orthopaedic/dental implants. Titanium and titanium alloy have been widely used in several bioimplant applications, but when implanted into the human body, these still contain some disadvantages, such as poor osteointegration (forming a fibrous capsule), wear debris and metal ion release, which often lead to clinical failure. Electrolytic hydroxyapatite/titanium dioxide (HA/TiO₂) double layers were successfully deposited on titanium substrates in TiCl₄ solution and subsequently in the mixed solution of Ca(NO₃)₂ and NH₄H₂PO₄, respectively. After annealing at 300∘C for 1 h in the air, the coated specimens were evaluated by dynamic cyclic polarization tests, immersion tests, tensile tests, surface morphology observations, XRD analyses and cells culture. The adhesion strength of the HA coating were improved by the intermediate coating of TiO₂ from 11.3 to 46.7 MPa. From cell culture and immersion test results, the HA/TiO₂ coated specimens promoted not only cells differentiation, but also appeared more bioactive while maintaining non-toxicity.     

The microwave effect on the properties of silica-coated TiO2 fine particles prepared using sol-gel method

The silica coating of TiO₂ fine particle was conducted using microwave assisted sol-gel method and conventional sol-gel method to suppress its photo-catalytic activity. The amount and uniformity of silica coating on TiO₂ surface were characterized by X-ray photoelectron spectroscopy (XPS), X-ray fluorescence spectroscopy (XRF), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and zeta potential measurements. XPS and XRF results showed that the presence of catalyst and reaction time were important factors to reach high silica amounts. SEM, TEM, and zeta potential results indicated that dense film coating of SiO₂ layer formed on TiO₂ surface in conventional sol-gel method, whereas the nucleation coating was observed on sample prepared by microwave assisted sol-gel method. When photo-catalytic activities and ultraviolet (UV) shielding abilities of these samples were evaluated, the sample prepared by microwave processing showed higher inhibition of photo-catalytic activity and better UV shielding ability than the sample prepared by conventional method. These results suggested that the coating method significantly affected the photo-catalytic activity and UV shielding ability of coated TiO₂.     

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.     

Synthesis and characterization of pure anatase TiO<Subscript>2</Subscript> nanoparticles

Pure anatase TiO₂ nanoparticles were synthesized by microwave assisted sol–gel method and further characterized by powder X-ray diffraction (XRD), energy dispersive x-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV–Visible spectrophotometer, SEM images showed that TiO₂ nanoparticles were porous structure. The XRD patterns indicated that TiO₂ after annealed at 300 °C for 3 h was mainly pure anatase phase. The crystallite size was in the range of 20–25 nm, which is consistent with the results obtained from TEM images. Microwave heating offers several potential advantages over conventional heating for inducing or enhancing chemical reactions.     

Two-step template-free route for synthesis of TiO<Subscript>2</Subscript> hollow spheres

The TiO₂ hollow microspheres were prepared by microwave-assisted solvothermal treatment without template. The morphology and the phase of TiO₂ hollow microspheres were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HR-TEM), and BET surface areas. The results show that the particles have hollow structures and the shell was covered by nanocrystals and have higher specific surface area. The possible formation mechanism of hollow TiO₂ spherical structures has simply been proposed. The activity was evaluated by the photocatalytic degradation of methyl orange (MO). The results show that the particles having specific surface area show higher photocatalytic activity. It can be attribute to the doped F atoms and the creation of oxygen vacancies.     

Fabrication of SiO<Subscript>2</Subscript>/TiO<Subscript>2</Subscript> double layer thin films with self-cleaning and photocatalytic properties

Transparent antireflective SiO₂/TiO₂ double layer thin films were prepared using a sol–gel method and deposited on glass substrate by spin coating technique. Thin films were characterized using XRD, FE-SEM, AFM, UV–Vis spectroscopy and water contact angle measurements. XRD analysis reveals that the existence of pure anatase phase TiO₂ crystallites in the thin films. FE-SEM analysis confirms the homogeneous dispersion of TiO₂ on SiO₂ layer. Water contact angle on the thin films was measured by a contact angle analyzer under UV light irradiation. The photocatalytic performance of the TiO₂ and SiO₂/TiO₂ thin films was studied by the degradation of methylene blue under UV irradiation. The effect of an intermediate SiO₂ layer on the photocatalytic performance of TiO₂ thin films was examined. SiO₂/TiO₂ double layer thin films showed enhanced photocatalytic activity towards methylene blue dye.     

Influence of O<Subscript>2</Subscript> Pressure on the Structure and Surface Morphology of YSZ Layer for YBCO Coated Conductor Deposited by PLD on Ni-W Tape

Yttria-stabilized ZrO₂ (YSZ) buffer layers were prepared on Ni-5%W tapes coated with CeO₂-seed layers by a pulsed laser deposition (PLD) technique. The influences of oxygen pressure on the structure and surface morphology of YSZ buffer layers for YBCO coated conductors was investigated. X-ray diffraction (XRD), scanning electron microscopy (SEM) and Atomic Force Microscope (AFM) were used to characterize YSZ films. It was found that the structure and surface morphology were sensitive to the oxygen pressure. When the O₂ pressure was higher than 1 mTorr, the YSZ film had mixed orientation and rugged surface. When the oxygen pressure was reduced to 0.5 mTorr, YSZ film had the pure (001) orientation. The surface became smooth as the oxygen pressure decreased. However, when the pressure was low to 0.1 mTorr, X-ray diffraction peaks form YSZ (002) were weak and the rough surface appeared again. The results could be explained either by plume stoichiometric changes, gas and ions interaction, or atomic rearrangement on the substrate.