Preparation and antibacterial activities of undoped and palladium doped titania nanoparticles

Undoped and palladium doped titania nanoparticles have been prepared by sol–gel method using isopropyl alcohol as solvent. The products have been characterized through XRD, FESEM, TEM, HRTEM, FTIR, specific surface area analysis and ICPOES technologies. The antibacterial activities of the products against Escherichia coli (E. Coli) have been investigated by microcalorimetric method and antibacterial circle method, respectively. The process of E. Coli growth and metabolism affected by nanoparticles has been monitored using a Thermal Activity Monitor (TAM) Air Isothermal Calorimeter by microcalorimetric method. The results indicate that undoped and palladium doped titania nanoparticles present better antibacterial activities. Among them, 3 mol% Pd doped titania nanoparticles exhibit the best antibacterial activity due to the lowest value of minimum inhibitory concentration (MIC). This result is in accordance with that of the antibacterial circle method. This work provides a general analytic technology to quantification study antibacterial activity of nanomaterials against various bacteria by microcalorimetric method, which could be a potential application in the future.     

Interaction of water with titania: implications for high-temperature gas sensing

High-temperature gas sensors based on semiconducting metal oxides show potential for optimization of combustion processes, resulting in efficient energy use and minimization of emissions. Such metal oxides can function as gas sensors because of the reaction of the sensing gas (e.g., CO) with ionosorbed oxygen species on the oxide surface with the resulting increase in conductivity. A limitation of metal oxide sensors is their difficulty of distinguishing between different gases. Designing selectivity into sensors necessitates a better understanding of the chemistry of gas-solid interactions at high temperatures. In this paper, we have used in situ infrared spectroscopy to monitor the dehydration of a hydrated anatase surface up to 600 degrees C and also to examine the hydration/dehydration of anatase held at 400 degrees C. When the O-H stretching region (3000-3800 cm(-1)) was primarily focused on, it was found that water loss from the titania surface proceeded at lower temperatures (<200 degrees C) through desorption, whereas at higher temperatures, water dissociation to terminal (approximately 3710 cm(-1)) and bridged (approximately 3660 cm(-1)) hydroxyl groups was noted. With a further increase in temperature to 600 degrees C, the bridged hydroxyl groups disappeared faster than the terminal ones. The electrical resistance of anatase at 600 degrees C was measured in the presence of moist gas streams and resulted in an increase in conductivity in the presence of water. In situ vibrational spectroscopy indicated a temporal correlation between the appearance of the bridging hydroxyl group and the change in electrical resistance. Several possible mechanisms are discussed. The chemical reaction of water with anatase at high temperatures necessitates that water be removed from the gas stream to avoid interference. A strategy involving the use of a hydrophobic microporous filter that can reject water and let gases such as CO pass unimpeded is examined. Successful use of such a concept has been demonstrated with a silicalite filter using moist CO gas streams.     

Preparation, phase transformation and photocatalytic activities of cerium-doped mesoporous titania nanoparticles

Cerium-doped mesoporous TiO₂ nanoparticles with high surface area and thermal stable anatase wall were synthesized via hydrothermal process in a cetyltrimethylammonium bromide (CTAB)/Ti(SO₄)₂/Ce(NO₃)₄/H₂O system. The obtained materials were characterized by XRD, FESEM, HRTEM, FTIR spectroscopy, nitrogen adsorption and DRS spectra. Experimental results indicated that the doping of cerium not only increased the surface area of mesoporous TiO₂ nanoparticles, but also inhibited the mesopores collapse and the anatase-to-rutile phase transformation. Moreover, the undoped, doped anatase mesoporous nanoparticles exhibit higher photocatalytic activity than commercial photocatalyst (Degussa, P25), but the maximum photodegradation rate corresponds to the undoped mesoporous TiO₂ nanoparticles. The lower photocatalytic activities of cerium-doped samples compared with undoped one may be ascribed to that the doped cerium partially blocks titania's surface sites available for the photodegradation and absorption of Rhodamine B (RB).     

Preparation and photocatalytic activity of multi-modally macro/mesoporous titania

Hierarchically disorder sponge-like macro/mesoporous titania was prepared by adding distilled water dropwise to a coating of tetrabutyl titanate. The results reveal that the un-calcined samples show obvious photocatalytic activity and multi-modal pore-size distribution. With increasing calcination temperatures, the photocatalytic activity and crystallinity increase. At 400°C, the calcined sample shows the highest photocatalytic activity. Further increasing the calcination temperatures results in the decrease of photocatalytic activity due to the drastic decrease of specific surface areas. However, the 600°C-calcined sample exhibits the highest specific photocatalytic activity due to high anatase crystallinity.     

Preparation of montmorillonite/titania nanocomposite and enhanced electrorheological activity

We prepared a new type of electrorheological particle composed of TiO2 nanocrystallites-coated montmorillonite (MMT/TiO2) nanocomposite by the sol-gel technique. The characterizations including TGA, XRD, TEM, SEM, EDS, and FTIR showed that TiO2 was deposited on the surface of the MMT flakes with anatase nanocrystallite. An obviously enhanced ER effect was found in the MMT/TiO2 nanocomposites based ER fluids compared with pure MMT and TiO2. Furthermore, the temperature and sedimentation stabilities of the MMT/TiO2 ER fluids had also been improved greatly. Interestingly, the content of TiO2 was demonstrated to have an important influence on the ER effect. When the content of TiO2 was about 20 wt%, the ER effect of MMT/TiO2 ER fluid reached its maximum, which was about 5 times that of pure MMT ER fluid and 27 times that of pure TiO2 ER fluid. Based on dielectric analysis, the significant ER enhancement by formation nanocrystallites-coated montmorillonite was attributed to the enhanced interfacial polarization in this nanocomposite particle due to the effective limitation of the long-range drift of active ions in montmorillonite particles.     

Application of Pt@SnO2 nanoparticles for hydrogen gas sensing

We report the fabrication of Pt@SnO₂ nanoparticles using a sol–gel method. These nanoparticles are used as a sensing material. The structural and morphological characterization of the prepared Pt@SnO₂ nanoparticles was performed using ultraviolet–visible spectroscopy, X‐ray diffraction, transmission electron microscopy, and energy‐dispersive X‐ray spectroscopy. The sensor responses of SnO₂ and 1 wt% Pt/SnO₂ to 1% hydrogen gas (H₂) were 1.3 and 1.9, respectively. The sensor response of a Pt@SnO₂ core–shell sensor increased to 5.1 at room temperature; it improved by 3.9 times compared to SnO₂ and by 2.7 times compared to 1% Pt/SnO₂ in sensing 1% H₂. The response time for the prepared Pt@SnO₂ sensor was also shortened by 2.0 and 1.4 times compared to SnO₂ and 1 wt% Pt/SnO₂, respectively. The sensor response increased rapidly from 1.4 to 5.1, with an increase in H₂ concentration from 800 to 10,000 ppm (1%). We investigated the H₂‐sensing mechanism of Pt@SnO₂.     

Photocatalytic activity of Fe and Cu co-doped TiO2 nanoparticles under visible light

Journal of Sol-Gel Science and Technology - The photocatalytic activity of single transition metal-doped TiO2 nanoparticles is well established. This article reports the synthesis of Fe and Cu...     

Morphology and photoluminescence study of titania nanoparticles

Titania nanoparticles are prepared by sol–gel chemistry with a poly(ethylene oxide) methyl ether methacrylate-block-poly(dimethylsiloxane)-block-poly(ethylene oxide) methyl ether methacrylate triblock copolymer acting as the templating agent. The sol–gel components—hydrochloric acid, titanium tetraisopropoxide, and triblock copolymer—are varied to investigate their effect on the resulting titania morphology. An increased titania precursor or polymer content yields smaller primary titania structures. Microbeam grazing incidence small-angle X-ray scattering measurements, which are analyzed with a unified fit model, reveal information about the titania structure sizes. These small structures could not be observed via the used microscopy techniques. The interplay among the sol–gel components via our triblock copolymer results in different sized titania nanoparticles with higher packing densities. Smaller sized titania particles, (∼13–20 nm in diameter) in the range of exciton diffusion length, are formed by 2% by weight polymer and show good crystallinity with less surface defects and high oxygen vacancies.     

Preparation and photocatalytic activity of visible light-active sulfur and nitrogen co-doped SrTiO3

Nitrogen and sulfur co-doped SrTiO₃ was prepared by high energy grinding of the mixture of SrTiO₃ and thiourea. A new band gap in visible light region (522 nm) corresponding to 2.37 eV could be formed by the co-doping. The photocatalytic activity for nitrogen monoxide oxidation of SrTiO₃ in visible light region especially in the long wavelength range (λ > 510 nm) could be improved greatly. Under the irradiation of light with wavelength larger than 510 nm, the photocatalytic activity of nitrogen and sulfur co-doped SrTiO₃ was 10.9 times greater than that of pure SrTiO₃. The high visible light photocatalytic activity of this substance may be due to the formation of a new band gap that enables to absorb visible light effectively.     

Synthesis,magnetic and ethanol gas sensing properties of semiconducting magnetite nanoparticles

The superparamagnetic magnetite (Fe₃O₄) nanoparticles with an average size of 7 nm were synthesized using a rapid and facile microwave hydrothermal technique. The structure of the magnetite nanoparticles was characterized by X-ray diffraction (X-ray), field effect scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The prepared Fe₃O₄ was shown to have a cubic phase of pure magnetite. Magnetization hysteresis loop shows that the synthesized magnetite exhibits no hysteretic features with a superparamagnetic behavior. The ethanol gas sensing properties of the synthesized magnetite were investigated, and it was found that the responsibility time is less than 10 s with good reproducibility for ethanol sensor. Accordingly, it is evaluated that the magnetite nanoparticles can be effectively used as a solid state ethanol sensor in industrial commercial product applications.     

Fabrication and characterization of multi-metal co-doped titania films for a water-splitting reaction

Anchored visible-light-absorbing TiO(2) films have been synthesized by the layer-by-layer method on a quartz slide substrate as a new class of visible light-sensitive photocatalyst. UV-vis, XRD and XPS spectra show that W and Mn enter the TiO(2) lattices and partially substitute for Ti, and that W appears to have a solubility limit into the anatase structure. The Mn and W dopants cause new electronic states above the valence-band edge of pure TiO(2), and the new electronic states may be directly related to the visible-light absorption of doped TiO(2) films. A constant H(2) generation rate is obtained for long periods of time for all the investigated TiO(2) films, and the H(2) production rates for titania films doped with 0.74 at% W (relative to Ti) are 4.1 and 3.3 times higher than that of non-doped TiO(2) under UV and visible light, respectively, as the dopant atoms not only restrict the band gap to the visible region, but also facilitate the detrapping of charge carriers to the surface of the catalyst.     

Particle size, shape and activity for photocatalysis on titania anatase nanoparticles in aqueous surroundings

TiO(2) nanoparticles have been widely utilized in photocatalysis, but the atomic level understanding on their working mechanism falls much short of expectations. In particular, the correlation between the particle structure and the photocatalytic activity is not established yet, although it was observed that the activity is sensitive to the particle size and shape. This work, by investigating a series of TiO(2) anatase nanoparticles with different size and shape as the photocatalyst for water oxidation, correlates quantitatively the particle size and shape with the photocatalytic activity of the oxygen evolution reaction (OER). Extensive density functional theory (DFT) calculations combined with the periodic continuum solvation model have been utilized to compute the electronic structure of nanoparticles in aqueous solution and provide the reaction energetics for the key elementary reaction. We demonstrate that the equilibrium shape of nanoparticle is sensitive to its size from 1 to 30 nm, and the sharp crystals possess much higher activity than the flat crystals in OER, which in combination lead to the morphology dependence of photocatalytic activity. The conventionally regarded quantum size effect is excluded as the major cause. The physical origin for the shape-activity relationship is identified to be the unique spatial separation/localization of the frontier orbitals in the sharp nanoparticles, which benefits the adsorption of the key reaction intermediate (i.e., OH) in OER on the exposed five-coordinated Ti of {101} facet. The theoretical results here provide a firm basis for maximizing photocatalytic activity via nanostructure engineering and are also of significance for understanding photocatalysis on nanomaterials in general.     

金纳米粒子在TiO2气凝胶基质上的行为: 光催化活性评价和结构研究

TiO2 -Au aerogels containing different amounts of gold nanoparticles of different sizes (5 and 16 nm) were successfully synthesized using a sol-gel procedure, and were tested for salicylic acid photodegradation under UV irradiation. The structure and morphology of the obtained materials were investigated using X-ray diffraction, transmission electron microscopy, and N2 adsorption-desorption measurements. UV-Vis spectroscopy was used to study the optical properties. The effects of the gold nanoparticles on the TiO2 crystallization process were twofold, as follows: (i) the number of crystallized zones was strongly related to the concentration of the gold nanoparticles, and (ii) the smaller gold particles increased the time taken for the crystallization of the samples. It was found that the noble metal-doped samples exhibited higher degradation rates compared with bare titania. It was found that the most active photocatalyst in each studied system was the sample with the highest concentration of gold nanoparticles. Additionally, the highest degradation rate value was obtained with the smallest Au nanoparticles (46.4 10-3 μmol/(L·s).     

Preparation and characterization of porous C-modified anatase titania films with visible light catalytic activity

Visible-light-activated C-modified anatase titania films have been synthesized from TiCl₄ and carbonic ink by using the sol–gel route. The synthesized photocatalysts were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and optical measurements. The modifying carbon not only produces homogeneous worm-like structure with uniform pores, but also extends the absorbance spectra of the as-prepared films into visible region. The results of visible-light-induced degradation of methyl orange (MO) show that the C-modified titania films exhibits much higher photocatalytic activities than that of pure titania film prepared at the same conditions.     

氧化镁表面修饰稀土催化材料的制备和气敏性能

本文采用湿化学过程的柠檬酸络合法、可控化学沉淀法和溶胶-凝胶法合成了纳米复合金属氧化物LaFeO3,利用各种分析方法对材料的物性和结构进行了分析和表征;并测定了材料对氧化性气体和还原性气体的气敏性能．研究结果表明LaFeO3复合物对NO2在350℃灵敏度高达127．83,特别通过添加MgO对基材进行表面修饰灵敏度提高到845．37,约添加前的70倍．本文还进一步考察了添加质和添加量对基材的结构和气敏性能的影响,并通过研究材料表面对气体的吸脱附性能和元素电子结合能的变化对敏感作用机制进行了深入分析和探讨．     

Preparation,characterization and catalytic activity of biomaterial-supported copper nanoparticles

Synthesis of copper nanoparticles was carried out with nanocrystalline cellulose (NCC) as a support by reducing CuSO₄·5H₂O ions using hydrazine. Ascorbic acid and aqueous NaOH were also used as an antioxidant and pH controller, respectively. The synthesized copper nanoparticles supported on NCC (CuNPs@NCC) were characterized by UV–vis, XRD, TEM, XRF, TGA, DSC, N₂ adsorption-desorption method at 77 K and FTIR. The UV–vis confirmed the formation and stability of the CuNPs, which indicated that the maximum absorbance of CuNPs@NCC was at 590 nm due to the surface plasmon absorption of CuNPs. Morphological characterization clearly showed the formation of a spherical structure of the CuNPs with the mean diameter and standard deviation of 2.71 ± 1.12 nm. Similarly, XRD showed that the synthesized CuNPs@NCC was of high purity. The thermal analysis showed that the CuNPs@NCC exhibited better thermal behaviors than NCC. BET surface area revealed that the N₂ adsorption–desorption isotherms of CuNPs@NCC featured a type IV isotherm with an H3 hysterisis loop. This chemical method is simple, cost effective, and environmentally friendly. Compared to NCC-supported CuNPs and unsupported CuNPs, the as-prepared CuNPs@NCC exhibit a superior catalytic activity and high sustainability for the reduction of methylene blue with NaBH₄ in aqueous solution at room temperature. The CuNPs@NCC achieved complete reduction of MB with completion time, rate constant and correlation coefficient (R ²) of 12 min, 0.7421 min^?1 and 0.9922, respectively.     

高纯纳米氧化钛的制备及催化活性

以工业级硫酸钛为原料,在酸性环境下以EDTA作为络合剂,采用控制沉淀法制备高纯度纳米TiO2。考察了pH值、反应温度、煅烧温度等工艺条件对TiO2颗粒晶型、大小和分布影响。利用TEM、XRD、ICP等手段对产物进行表征,TiO2纯度超过99.9%,粒径为10-20nm,分布均匀。经过对其光催化降解苯酚反应活性实验,结果表明样品具有较好的光催化活性。     

Biomimetic synthesis of titania nanoparticles induced by protamine

Protamine, a kind of cationic protein extracted from sperm nuclei, was employed for the first time in vitro to induce the formation of a titania/protamine nanoparticle composite from a water-stable titanium precursor, titanium(iv) bis(ammonium lactato) dihydroxide (Ti-BALDH). The resulting titania/protamine nanoparticle composite was extensively characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). The titania/protamine nanoparticle composite was of amorphous structure, and exhibited a different morphology from those prepared by an alkali-catalyzed approach. The catalyzing and templating function of protamine involved in the synthesis of the nanoparticle composite is discussed, and a mechanism tentatively proposed. In addition, the effects of pH and temperature on the amount and size of as-prepared titania/protamine nanoparticle composite were systematically investigated.