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.     

The effects of synthesis procedures on the morphology and photocatalytic activity of multi-walled carbon nanotubes/TiO(2) nanocomposites

This study investigates the microstructures of multi-walled carbon nanotubes (MWNTs)/TiO(2) nanocomposites, obtained by sol-gel and hydrothermal processes. The synthesized nanocomposite materials were characterized by x-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) adsorption analysis, transmittance electron microscopy (TEM), scanning electron microscopy (SEM), photoluminescence (PL) spectroscopy, and x-ray photoelectron spectroscopy (XPS). The effects of the synthetic procedures and MWNTs on the morphology and photocatalytic activity of the nanocomposites were studied. The photocatalytic activity of the MWNTs/TiO(2) nanocomposite was elucidated based on the photooxidation of NO(x) under UV light illumination. A fleck-like and well dispersed TiO(2) microstructure on the surface of the MWNTs was observed in the sol-gel system, while compact and large aggregated particles were found in the hydrothermal procedure. The nanocomposite prepared by the sol-gel system exhibits better photocatalytic activity for NO oxidation (from 20.52 to 32.14%) than that prepared by the hydrothermal method (from 22.58 to 26.51%) with the same MWNT loading (from 0 to 8?wt%), respectively. The optimal MWNT content in the nanocomposite was considered at 8?wt%. Additionally, results confirm that the introduction of MWNTs will cause the NO(2) to be more consumed than NO in the photocatalytic experiments, leading to more complete NO(x) photooxidation. These observations indicate that the different TiO(2) distributions on the MWNT surfaces and MWNT contents in the materials would determine the morphology, the physicochemical and photocatalytic characteristics for the nanocomposite materials.     

Preparation polystyrene/multiwalled carbon nanotubes nanocomposites by copolymerization of styrene and styryl-functionalized multiwalled carbon nanotubes

Styryl-functionalized multiwalled carbon nanotubes (p-MWNTs) were prepared by esterification based on the carboxylate salt of carbon nanotubes and p-chloromethylstyrene in toluene. Then in situ radical copolymerization of p-MWNTs and styrene initiated by 2,2′-azobis(isobutyronitrile) (AIBN) was applied to synthesize composites of styryl-functionalized multiwalled carbon nanotubes and polystyrene (PS) (p-MWNTs/PS). Characterizations carried out by FT-IR, ¹H NMR, UV–vis show that styryl group covalently bond to the surface of MWNTs. The results of UV showed that the solutions of p-MWNTs/PS in chloroform have the hyperchromic effect. Transmission electron microscopy (TEM) images of p-MWNTs/PS composites and scanning electron microscopy (SEM) images of fracture surface of p-MWNTs/PS composites showed the functionalized nanotubes had a better dispersion than that of the unfunctionalized MWNTs in the matrix. The results of thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) suggested that the thermal stability of p-MWNTs/PS composites improved in the presence of MWNTs.     

Cathodoluminescence of TiO2 nanotubes prepared by low-temperature anodization of Ti foils

We show that anodization of Ti sheets in an ethylene glycol and HF containing electrolyte at temperatures under 0 °C results in the formation of a self-arranged ordered porous structure at the top surface of the sample. This perforated surface structure initiates the growth of an ordered array of titania nanotubes. The inner diameter of nanotubes can be modified in a controlled fashion in the range from 10 nm to more than 250 nm through the change of the electrolyte temperature from −20 °C to + 50 °C. The spectral distribution of cathodoluminescence from a cluster of nanotubes clearly demonstrates the formation of resonator modes which are separated from each other by around 200 meV.     

Morphology controllable synthesis of TiO2 by a facile hydrothermal process

Titanium dioxide nanoparticles were prepared via a facile hydrothermal approach with titanium tetrabutoxide as a precursor under strongly acidic condition. The transmission electron microscopy results showed that novel flower-like, leaf-like, and rod-like TiO₂ nanoscale materials could be easily obtained by tailoring the concentration of the precursor and the reaction temperature. And the analysis from X-ray diffraction revealed that all the as-prepared products under different experimental conditions possessed a mixed crystal phase of anatase and rutile. The reasons for the phase formation were discussed. Larger proportion of rutile phase should be ascribed to the strongly acidic conditions. The growth mechanisms of TiO₂ nanostructures with various morphologies were also proposed.     

钛酸铋钠的水热合成与表征

采用水热法合成出(Na1/2Bi1/2)TiO3钙钛矿复合氧化物超细粉料,实验研究确定了最优合成过程参数矿化剂NaOH浓度为12mol/L前驱体溶液的pH值在12～13范围内、在180℃下反应48h,并制备出单一钙钛矿结构的NBT合成粉料.采用XRD、SEM等分析手段对合成粉体的结构、形貌进行了表征.分析结果表明合成的粉体为纯钙钛矿结构,粉体形貌大体呈现圆球状,颗粒大小比较均匀,直径分布在O.2～1.0μm范围,平均粒径为0.5um左右.与常规固相合成法相比,水热法制备的(Na1/2Bi1/2)TiO3陶瓷样品表现出较好的压电性能,其压电性能参数d33达到了82pC/N.     

Phase selection and visible light photo-catalytic activity of Fe-doped TiO2 prepared by the hydrothermal method

It is necessary to extend the absorption range of TiO₂ based materials from the ultraviolet to the visible light region for most photo-catalytic applications of TiO₂ under solar irradiance or indoor lighting. Also, the ability to control the structural evolution, particularly the competition and transformation between different phases (anatase or rutile), is extremely important for the preparation of high efficiency TiO₂ based photo-catalysts. In this work, we have systematically studied the effects of various processing factors on the phase selection process/outcome of nanocrystalline Fe-doped TiO₂, which includes the level of doping ions, annealing temperature, solution pH and the addition of acidic anions, using a low temperature hydrothermal method. Both Fe-doped rutile and anatase TiO₂ phases were obtained via varying the processing conditions. The visible-light photo-catalytic activity of doped materials was significantly improved over that of the pure TiO₂ nanopowders, which was demonstrated by effective degradation of methylene blue under visible light.     

Preparation and properties of the polyimide/multi-walled carbon nanotubes (MWNTs) nanocomposites

The polyimide/multi-walled carbon nanotubes (MWNTs) nanocomposite films were prepared by mixing of poly(amic acid) (PAA) solution and MWNTs/DMAc suspension follow by mixture casting, evaporation and thermal imidization. To increase the chemical compatibility between polyimide matrix and MWNTs, MWNTs were modified with mixed strong acid. The results show that the dispersion of the MWNTs is improved greatly in the polyimide matrix after acid modification. The modified MWNTs are dispersed homogeneously in the polyimide matrix while the structure of the polyimide and MWNTs structures is stable in the preparation process. With the incorporation of MWNTs, the mechanical properties of the resultant nanocomposite films were greatly improved due to the strong interfacial interaction between the modified MWNTs and the polyimide matrix. The thermal stability of the nanocomposites was lower a little than pure polyimide because of the drop of thermostability of MWNTs through acid-treatment. The electrical conductivity and the dielectric constant of the nanocomposites were also having sharp increase, which is favorable for practical use in anti-static materials and embedded capacitors.     

Studies on preparation and properties of the multi-walled carbon nanotubes (MWNTs)/epoxy nanocomposites

The MWNTs were coated with polyaniline (PANI) by in situ chemical oxidation polymerization method. FTIR spectroscopy, scanning electron microscope (SEM) and X-ray diffraction (XRD) indicated that the MWNTs were coated with PANI. The MWNTs/epoxy nanocomposites were fabricated by using the solution blending method. Differential scanning calorimetry (DSC), tensile testing, HP 4294A impedance analyzer and SEM were used to investigate the properties of the nanocomposites. The results showed that the modified carbon nanotubes were well dispersed in the polymer matrix. The nanocomposites have enhancements in mechanical, thermal and dielectric properties compare with the neat epoxy resin. The nanocomposites were proven to be a good polymer dielectric material.     

Ag surfactant effects of TiO2 films prepared by sputter deposition

The surfactant effect of Ag on the thin film structure of TiO₂ by radio frequency magnetron sputtering has been investigated. Comparisons between the atomic force microscopy images revealed that the surface roughness of TiO₂ film mediated by Ag was smaller than that of the TiO₂ film without Ag. The surface segregation effect of Ag was confirmed using X-ray photoelectron spectroscopy. The results of X-ray diffraction revealed that the initial deposition of a 0.4 nm thick Ag surfactant layer onto a Fe buffer layer prior to the deposition of the TiO₂ film reduced the rutile (110) growth and enhanced the anatase (100) growth. It was concluded that Ag was an effective surfactant for changing the thin film structure of TiO₂ on the Fe buffer layer. The photocatalytic effect of the fabricated TiO₂ film was also investigated using the remote oxidation process. TiO₂ films with the Ag surfactant exhibited higher photocatalytic activity than conventionally deposited TiO₂ films.     

原位复合法制备TiO2 / ( PEO)8LiClO4 聚合物电解质

以聚氧化乙烯/ 高氯酸锂络合物( ( PEO)₈LiClO₄ ) 为基体, 通过钛酸四丁酯的水解缩合反应在基体中原位生成TiO₂粒子, 制备了TiO₂ / ( PEO)₈LiClO₄复合聚合物电解质膜。采用SEM、DSC 和交流阻抗方法分别研究了电解质膜的表面形貌、热性能和离子导电性能。结果表明, 原位生成的TiO₂ 粒子均匀分散于PEO 基体中。复合TiO₂后电解质膜的玻璃化转变温度和结晶度降低。电解质膜的离子导电行为满足Arrhenius 方程, 并在5 %TiO₂含量时体系的电导率出现最大值5. 5 ×10 -5 S/ cm (20 ℃) 。以此膜为电解质组装的全固态聚合物锂电池放电时电压平稳, 20 次循环后放电容量保持在107 mAh/ g。      

Nanoporous TiO2 films prepared by thermal rapid treatment (TRT)

Nanoporous TiO₂ films were fabricated by thermal rapid treatment (TRT) of the TiO₂ film which was previously deposited on a substrate by liquid phase deposition. The TiO₂ films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and UV-VIS diffuse reflectance spectroscopy (UV-VIS DRS). Photocatalytic activity of nanoporous TiO₂ coating was assessed by the photocatalytic degradation of methylene blue aqueous solution.     

不同酸化条件下水热合成V2O5粉末的结构和电化学性能

为了研究酸化条件对V2O5粉末结构和电化学性能的影响,利用HNO3和H2C2O4酸化NH4VO3溶液,经水热和后续热处理制备了V2O5粉体。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和电化学工作站等对V2O5粉体的微观结构与电化学性能进行了测试。结果表明,所得粉体为纯V2O5相,前驱体溶液的pH值和酸化所用酸的酸根阴离子影响了最终粉体的晶体发育和微观结构。其中,利用HNO3酸化NH4VO3溶液至pH值=3制得的粉体为直径约100nm的纳米棒,在0.5和1C的放电速率下循环30次后,放电比容量仍有150mAh/g左右,且大电流放电性能更好。     

Photodecomposition effects of graphene oxide coated on TiO2 thin film prepared by electron-beam evaporation method

Morphological, structural and photocatalytic properties of graphene oxide (GO)/TiO₂ thin-film deposited on quartz substrate were investigated. The TiO₂ film was prepared by electron-beam evaporation and the GO film by spin coating method. The photocatalytic activities of the GO/TiO₂ film were evaluated by photodecomposition of methylene blue. There was synergistic effect between TiO₂ and GO which causes a rapid photo-induced charge separation and the reduction of the recombination of electron-hole pairs under the UV-visible light irradiation. GO on TiO₂ film also promotes the properties of adsorption of the dye, photon scattering probability, and interacting surface area. As a result, it leads to the enhancement of the efficiency of the photodegradation in GO/TiO₂ film.     

Properties of TiO2 prepared by acid treatment of BaTiO3

TiO₃ powders were prepared by acid treatment of BaTiO₃ and their properties were investigated. The BaTiO₃ powder was subjected to HNO₃ in concentrations ranging from 10⁻³ to 8 M at 90 °C for 0.5-6 h. Dissolution of BaTiO₃ and precipitation of TiO₂ occurred at acid concentrations of 2-5 M. BaTiO₃ dissolves completely to form a clear solution at reaction times of 0.5-1 h, but a rutile precipitate is formed after 2 h of acid treatment. By contrast, anatase is precipitated by adjusting the pH of the clear solution to 2-3 using NaOH or NH₄OH solution. The rutile crystals were small and rod-shaped, consisting of many small coherent domains connected by grain boundaries with small inclination angles and edge dislocations, giving them a high specific surface area (S_BET). With increasing HNO₃ concentration, the S_BET value increased from 100 to 170 m²/g while the crystallite size decreased from 25 to 11 nm. The anatase crystals obtained here were very small equi-axial particles with a smaller crystallite size than the rutile and S_BET values of about 270 m²/g (higher than the rutile samples). The photocatalytic activity of these TiO₂ was determined from the decomposition rate of Methylene Blue under ultraviolet irradiation. Higher decomposition rates were obtained with larger crystallite sizes resulting from heat treatment. The maximum decomposition rates were obtained in samples heated at 500-600 °C. The photocatalytic activity of the TiO₂ was found to depend more strongly on the sample crystallite size than on S_BET.     

Macroporous TiO2/carbon composites prepared via a simple soaking process

A new-type composite photocatalyst of three-dimensional ordered macroporous (3DOM) TiO₂/C was prepared and tested in this paper. 3DOM carbon materials were first prepared by colloidal crystal templating process, and then the sols of TiO₂ from tetrabutyl titanate were infiltrated in the macroporous structures via capillary force. After calcinations at nitrogen flow, TiO₂/C composite materials were prepared. The obtained samples were analyzed by SEM, TEM, XRD and BET. The results indicated that macroporous TiO₂/C can remain the three-dimensional ordered structure and TiO₂ nanoparticles distributed in the interior of macropores uniformly. Eventually, 3DOM TiO₂/C materials were used as a new-type photocatalysts to decompose the methyl orange solution under ultraviolet light, which displayed excellent catalytic activity and regenerative ability.     

Low-temperature and ambient-pressure synthesis of TiO2(B)

Nanocrystalline TiO₂(B) powder was obtained by the hydrolysis of an ionic liquid like titania precursor (the triethylammonium salt of hexafluorotitanate) induced by the addition of boric acid in the presence of dopamine. The entire synthetic procedure was carried out at ambient pressure and low temperature (85 °C). X-ray diffraction, high resolution transmission electron microscopy and selected area electron diffraction characterization techniques confirmed the formation of the TiO₂(B) phase. Moreover, Raman spectroscopy indicated that TiO₂(B) was the major component, although it also revealed the presence of anatase as a minor component (< 10%). The as-prepared material has a mesoporous architecture with high specific surface area (235 m² g^− 1).     

Photoactivity of anatase–rutile TiO2 nanotubes formed by anodization method

Titania (TiO₂) nanotubes were prepared by anodizing titanium (Ti) foils in an electrochemical bath consisting of 1 M glycerol with 0.5 wt.% NH₄F.The pH of the bath was kept constant at 6 and the anodization voltage was varied from 5 V, 20 V to 30 V. It is found that the morphology of the anodized titanium is a function of anodization voltage with pits-like oxide formed for the sample made at 5 V and samples made at 20 V and 30 V consisted of well-aligned nanotubes growing perpendicularly on the titanium foil. However, the nanotubes formed on the samples made at 30 V were not uniform in terms of the nanotubes' diameter and wall thickness. Regardless of the anodization voltage, as anodised samples were amorphous. The crystal structure evolution was studied as a function of annealing temperatures and was characterised by X-ray diffraction and Raman spectroscopy analyses. Crystallization of the nanotubes to anatase phase occurred at 400 °C while rutile formation occurred at 700 °C. Disintegration of the nanotube arrays was observed at 600 °C and the structure completely vanished at 700 °C. TiO₂ nanotube annealed at 400 °C and containing 100% anatase revealed the highest photocatalytic activity for the degradation of methyl orange. Consequently, these results indicate that diameter, wall thickness, crystal structure and degree of crystallinity of the TiO₂ nanotube arrays are the important factors influencing the efficiency of the photocatalytic activity.     

Facile synthesis of SnO2 nanograss array films by hydrothermal method

SnO₂ nanograss array films (SNAFs) were synthesized on indium tin oxide glass substrates by hydrothermal method. The effects of preparing conditions such as precursor concentration, reaction temperature and growth time on the formation of the SNAFs have been investigated in detail by scanning electron microscopy, high resolution transmission electron microscopy, X-ray diffraction and photoluminescence spectrum. It is shown that the precursor concentration plays an important role in determining the morphology of the prepared SnO₂. The average diameter, length and growth rate of the SNAFs can be controlled to some extent by varying growth time. The reaction temperature has also influence on the growth rate of SNAFs. Moreover, the growth mechanism of the SNAFs was also discussed. Room-temperature photoluminescence spectra were further carried out to investigate their optical properties.