Heat treatment on TiO2 nanoparticles prepared by vapor-phase hydrolysis

TiO₂ nanoparticles are prepared by vapor-phase hydrolysis of TiCl₄ below 550°C and are characterized by TEM, XRD and XPS before and after heat treatment at various temperatures. It shows that anatase/amorphous particles start to transform to rutile at certain temperature. Such transformation temperature tends to decrease with the decrease of particle size. When the rutile phase starts to be formed, the particles grow rapidly, while they grow slowly before the appearance of rutile titania. The Ti2p_3/2 binding energies tend to increase as particle sizes decrease, especially for particles below 50 nm in size.     

Characterization of the structures of size-selected TiO2 nanoparticles using X-ray absorption spectroscopy

To investigate the relationship between the size and structure of TiO(2) nanoparticles, three size-selected samples of TiO(2) nanoparticles were prepared via a hydrolysis method that uses Ti[OCH(CH(3))(2)](4) as the starting material. The structures of the nanoparticles were characterized using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray absorption spectroscopy (XAS). Analysis of the XRD patterns and of the TEM images showed that the samples were dispersed, with an average particle size of approximately 30 nm (sample A), approximately 12 nm (sample B), and approximately 7 nm (sample C). Their X-ray absorption spectra indicate that samples A and B have an anatase structure, whereas sample C has a structure very similar to that of the TiO( 2) II phase, which generally arises only under high-pressure conditions. This difference can be attributed to size-induced radial pressure within the smaller nanoparticles, which plays an important role in the phase of TiO(2) nanoparticles in sample C.     

Different methods in TiO2 photodegradation mechanism studies: gaseous and TiO2-adsorbed phases

The development of photocatalysis processes offers a significant number of perspectives especially in gaseous phase depollution. It is proved that the photo-oxidizing properties of photocatalyst (TiO(2)) activated by UV plays an important role in the degradation of volatile organic compounds (VOC). Heterogeneous photocatalysis is based on the absorption of UV radiations by TiO(2). This phenomenon leads to the degradation and the oxidation of the compounds, according to a mechanism that associates the pollutant's adsorption on the photocatalyst and radical degradation reactions. The main objective of the study is the understanding of the TiO(2)-photocatalysis phenomenon including gaseous and adsorbed phase mechanisms. Results obtained with three different apparatus are compared; gaseous phases are analysed and mechanisms at the gaseous phase/photocatalyst interface are identified. This study leads to improve understanding of various mechanisms during pollutant photodegradation: adsorption of pollutants on TiO(2) first takes place, then desorption and/or photodegradation, and finally, desorption of degradation products on TiO(2). The association of analytical methods and different processes makes the determination of all parameters that affect the photocatalytic process possible. Mastering these parameters is fundamental for the design and construction of industrial size reactors that aim to purify the atmosphere.     

Sonochemical preparation of TiO2 nanoparticles

TiO₂ nanoparticles with mean diameter of about 20 nm, average crystallite size of 15 nm and BET specific surface area of 78.88 m²/g, were prepared through a simple sonochemical method and initial treatment in 10 M NaOH aqueous solution. XRD results exhibited that the obtained nanoparticles composed of pure rutile phase. During the initial treatment with NaOH aqueous solution, the Ti–O–Ti bonds in the TiO₆ octahedra structure of the raw material were broken, and new octahedras formed after ultrasonic irradiation. It is supposed that edge sharing was favored during ultrasonic treatment, leading to formation of the rutile nanoparticles.     

Co-sedimentation of TiO2 nanoparticles and polymer beads to fabricate macroporous TiO2 photoelectrodes

Dye-sensitized solar cells based on highly porous nanocrystalline TiO2 films have drawn considerable attention due to their high conversion efficiency and low production cost. TiO2 nanocrystalline electrodes have been investigated extensively as a key material. In this study, we discuss dye-sensitized solar cells based on macroporous TiO2 films using a highly-dispersed aqueous solution of TiO2 nanoparticles and polymeric particles. After drying this solution on the conducting glass substrate, the sacrificial polymer particles were removed selectively by thermal sintering at high temperatures over 400 degrees C or chemical treatment at the low temperature of 150 degrees C. This method provides the flexible control of TiO2 fractions or pore size or fabrication temperature. Also highly-dispersed TiO2 particles with a high crystallinity would provide a promising solution on low-temperature process for flexible DSSCs.     

An organometallic synthesis of TiO2 nanoparticles

We report the synthesis of TiO2 nanoparticles that uses the low-temperature reaction of low-valent organometallic precursors. Bis(cyclooctatetraene)titanium reacts with dimethyl sulfoxide in organic solution at temperatures as low as room temperature to produce TiO2. In the absence of any supporting ligand, the reaction gives precipitation of amorphous TiO2 powder; however, in the presence of basic ligands such as tributylphosphine, tributylphosphine oxide and trioctylphosphine oxide, the precipitation is arrested, and chemically distinct, isolated, internally crystalline TiO2 nanoparticles are formed.     

纳米TiO2粉体的制备及其表征

采用溶胶-凝胶技术制备了纳米TiO2粉体,并对其热性能、相结构、颗粒大小和分布进行了表征,结果表明,TiO2干凝胶粉经300℃煅烧后已有锐钛矿相出现,经550℃煅烧后有金红石相出现,完全相转变的温度约为600℃,纳米TiO2粉体的颗粒尺寸随煅烧温度的升高而增大,采用溶胶,凝胶技术制备的干凝胶粉经400℃煅烧后可获得团聚轻、颗粒大小分布比较均匀、颗粒尺寸约为15nm的球状TiO2粉体,     

Analysis of optical properties of TiO2 nanoparticles and PAN/TiO2 composite nanofibers

The aim of the study was the production of thin composite nanofibrous mats PAN/TiO₂ nanoparticles using the electrospinning method from solution of PAN/TiO2/DMF. TiO₂ nanoparticles were obtained using sol-gel method. To prepare sol mixture, organic alkoxides precursor of titanium isopropoxide and water solution were used. Calcination of TiO-gel and following milling were carried out to obtain nanoparticles of TiO₂ rutile phase. In order to analyze the structure of the obtained particles, we used X-ray diffraction analysis (XRD) and energy dispersive spectrometer (EDS). Analysis of the morphology and chemical composition of the resulting composite nanofibers were carried out using a scanning electron microscope (SEM) with EDS. The analysis of the optical properties and the energy band structure prepared nanoparticles and thin composite nanofibrous mats were determined by spectral analysis of the absorbance as a function of the energy of radiation obtained using a UV–Vis spectrophotometer.     

Characterization of Sol-gel-derived TiO2 and TiO2-SiO2 Films for Biomedical Applications

In order to improve the corrosion resistance and biocompatibility of NiTi surgical alloy, TiO2 and TiO2-SiO2 thin films were prepared by sol-gel method. The surface characteristics of the film, which include surface composition, microstructure and surface morphology, were studied by X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectra (XPS), respectively. A scratching test was used to assess the interface adhesive strength between the film and substrate. The corrosion resistance of NiTi alloy coated with oxide films were studied by anodic polarization curves measurement in biological solution. Additionally, a preliminary study of the in vitro bioactivity of the films was conducted. The results indicated that TiO2 and TiO2-SiO2 (Ti/Si=4:1) films have higher electrochemical corrosion resistance and can be used as protective layers on NiTi alloy. In addition, TiO2-SiO2 composite films have better bioactivity than TiO2 film.     

铁掺杂纳米TiO2的制备及其光催化性能研究

采用溶胶-凝胶法制备了掺杂Fe3 的纳米TiO2微粒,采用X光衍射仪对粉体进行了表征.以甲基橙为目标降解物,研究了Fe3 掺杂纳米TiO2光催化性能.结果表明,掺杂适量Fe3 能够提高TiO2的光催化活性,当Fe3 的掺入量为摩尔比0.41%时催化活性最高.以紫外灯为光源,降解初始浓度为20mg·L-1的250mL甲基橙溶液,催化剂0.41%(摩尔分数)Fe3 -TiO2投加量为0.5g时,甲基橙的光催化降解效果最好.     

Laser-assisted production of spherical TiO2 nanoparticles in water

TiO(2) nanoparticles with controllable average diameter have been obtained by laser ablation in water. A monomode ytterbium doped fiber laser (YDFL) was used to ablate a metallic titanium target placed in deionized water. The resulting colloidal solutions were subjected to laser radiation to study the resizing effect. The crystalline phases, morphology and optical properties of the obtained nanoparticles were characterized by means of transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), x-ray energy dispersive spectroscopy (EDS) and UV-vis absorption spectroscopy. The colloidal suspensions produced consisting of titanium dioxide crystalline nanoparticles show almost perfect spherical shape with diameters ranging from 3 to 40 nm. The nanoparticles are polycrystalline and exhibit anatase as well as rutile phases.     

氮掺杂空心TiO2纳米粒子的制备与研究

采用一种简便的方法合成了氮掺杂空心TiO:纳米粒子.以聚苯乙烯(PS)纳米粒子为模板、氨水为催化剂、三乙醉胺为抑制剂,采用溶胶-凝胶方法合成了PS/TiOZ(核/壳)纳米复合粒子.考察了氨水、三乙醉胺和钛酸正丁酯用量对TiO:壳层表面形态和厚度的影响.氨水用量3.OOg时TiO2壳层表面较光滑,氨水用量6.OOg时其表...     

Photocatalytic activity of TiO2-capped ZnO nanoparticles

Using a combined hydrothermal and sol–gel route, TiO₂ -capped ZnO nanoparticles with an average size of 60 nm were prepared. The titania shell was amorphous with a thickness of ~10 nm. Formation of Zn₂TiO₄ phase at higher calcination temperature was noticed. Effects of Ti/Zn molar ratio and coating time on the thickness of TiO₂ shell and the photoactivity of the particles for decolorization of Methylene Blue (MB) under UV lamp irradiation (3 mW/cm²) were investigated. The nanoparticles were characterized by X-ray diffraction, transmission electron microscopy, fourier-transform infrared spectrometry (FTIR), diffuse reflectance spectroscopy (DLS), and atomic absorption spectroscopy. Analysis of the photoactivity results according to Langmuir–Hinshelwood model revealed a two-step decolorization process with a high kinetics rate at the early stage followed by a slower step. The capped nanoparticles synthesized under specific conditions exhibited higher photodecolorization yield and faster kinetics in comparison to the uncoated ZnO and P25-Degussa TiO₂ nanoparticles.     

纳米TiO2粉体的低温制备

采用液相沉积法制备锐钛矿型TiO2纳米光催化粉体,研究了沉积温度、反应物的摩尔比、沉积时间、[TiF6]^2-水溶液的浓度等对TiO2粉体性能的影响。用甲基橙的光催化降解表征了所制备的TiO2粉体的光催化活性。结果表明光催化活性最佳的实验参数为：温度为90℃,(NH4)2TiF6与H3BO3的摩尔比为1：2。5,沉积时间为1h,加水量为320ml。     

纳米TiO2粉体的制备与性能表征

以硫酸法生产钛白粉的中间产物偏钛酸为原料，利用盐酸溶解-氨水中和沉淀法，成功地制备了纳米锐钛矿型TiO2，并采用热重分析、X射线衍射、透射电镜等技术研究了纳米粉体材料的晶型结构和形貌特征。实验结果表明：所制的前驱体水合TiO2粉体本身已具锐钛矿型，经600℃煅烧后粉体结晶性较好仍为锐钛矿型，平均颗粒粒径大小为20nm。     

氧化钛纳米管的合成机理与表征

采用水热合成方法制备出外径约8nm,壁厚为1nm的纳米管,以TEM、XRD和TG等分析手段对不同工艺条件下获得的产物进行了表征,对它们的热稳定性进行了测试。结果表明,纳米管是在NaOH水热处理过程中形成的,而不是在清洗过程中形成的。其形成机理可能是纳米氧化钛颗粒在强碱作用下形成的Na2TiO3片状物经过卷曲而成短纳米管,通过溶解-吸收机理,逐渐长成长纳米管。但清洗溶液的pH值对生成的纳米管的成分和结构有影响,通过控制清洗产物溶液的pH值和热处理温度,可以获得组成分别为Na2TiO3、H2TiO3和TiO2的纳米管,且纳米管具有较好得热稳定性,经400℃热处理后,能保持其纳米管形貌,600℃时,纳米管间有烧结的迹象,至800℃时纳米管完全变为颗粒状。     

Phase-pure TiO(2) nanoparticles: anatase, brookite and rutile

We report on the synthesis of phase-pure TiO(2) nanoparticles in anatase, rutile and brookite structures, using amorphous titania as a common starting material. Phase formation was achieved by hydrothermal treatment at elevated temperatures with the appropriate reactants. Anatase nanoparticles were obtained using acetic acid, while phase-pure rutile and brookite nanoparticles were obtained with hydrochloric acid at a different concentration. The nanomaterials were characterized using x-ray diffraction, UV-visible reflectance spectroscopy, dynamic light scattering, and transmission electron microscopy. We propose that anatase formation is dominated by surface energy effects, and that rutile and brookite formation follows a dissolution-precipitation mechanism, where chains of sixfold-coordinated titanium complexes arrange into different crystal structures depending on the reactant chemistry. The particle growth kinetics under hydrothermal conditions are determined by coarsening and aggregation-recrystallization processes, allowing control over the average nanoparticle size.     

Synthesis and investigations of rutile phase nanoparticles of TiO2

TiO₂ nanoparticles have been synthesized at room temperature using a simple chemical precipitation route. Particles were further coated with polymer. Detailed structural analysis of the particles has been carried out. Wide-angle X-ray scattering (WAXS) and transmission electron microscopy (TEM) confirm that as-synthesized particles as well as annealed particles are nanoparticles having pure rutile phase. Thermal annealing at 1000 °C of 4.2 nm particles led to an increased size 20 nm in the same phase. The purity and composition of the particles were determined using energy dispersive analysis of X-rays (EDAX) and X-ray photoelectron spectroscopy (XPS), respectively.