Nitrogen-doped and gold-loaded TiO2 photocatalysts synthesized by sequential reactive pulsed laser deposition

Nitrogen-doped titanium oxide thin films covered by gold metal nanoparticles were grown on (001) SiO₂ quartz substrates by pulsed laser deposition. A KrF* excimer laser source (λ = 248 nm, τ _FWHM ≤ 25 ns, ν = 10 Hz) was used for the irradiation of TiO₂ and gold metal targets. The experiments were performed in controlled reactive oxygen or nitrogen atmosphere. The layers were grown for photocatalytic applications. Evaluation of photocatalytic activity was performed by photodegradation of methyl orange under near-UV light irradiation. Our results show that nitrogen doping and addition of gold nanoparticles have complementary effects, photoactivity being significantly improved as compared to that of pure titanium oxide.     

Modernized H2S-treatment of TiO2 nanoparticles: Improving quantum-dot deposition for enhanced photocatalytic performance

One of the efficient strategies to enhance light harvesting capability of metal oxides nanoparticles (NPs) is to deposit low band gap metal sulfides on them via pseudo-successive ionic layer adsorption and reaction (p-SILAR). Resultant oxide-sulfide nanocomposites have a variety of applications, however there is still a need to increase the deposition of metal sulfide in the form of quantum-dots (QDs). In this work, we have successfully enhanced the deposition of QDs on TiO₂ NPs using a modernized H₂S-treatment strategy. A rotary reactor was employed for H₂S-treatment of TiO₂ NPs, ensuing higher deposition of PbS (in TiO₂–PbS) and CdS (in TiO₂–CdS) via p-SILAR. Resultantly, dye degradation of Rhodamine B increased from 63% to 75% and 72%–84%, respectively. X-ray photoelectron spectroscopy revealed the efficacy of modernized H₂S-treatment while intensive electrochemical characterization affirmed reduction in charge carrier transfer resistances due to superior deposition of PbS and CdS QDs on TiO₂ NPs.     

用SAXS和XRD方法研究Ti02纳米颗粒微观结构

用溶胶一凝胶方法制备了TiO2纳米样品.并对该样品在300℃到800℃温度区域进行了退火处理.应用同步辐射x射线粉未衍射(XRD)方法研究了经不同热处理温度的TiO2纳米颗粒的结构相变.应用同步辐射小角x射线散射(SAXS)方法研究了TiO2纳米颗粒的表面分形与界面特性.得到纳米颗粒粒度与退火温度的变化规律,讨论r表面界面特征与相变的关系.     

Synthesis and characterization of composite Au/TiO2 nanoparticles by laser irradiation

Composite Au/TiO₂ nanoparticles were synthesized by laser ablation of gold plate in TiO₂ sol. The nanoparticles were characterized by UV-visible spectroscopy, transmission electron microscopy, X-ray diffraction, and atomic force microscopy. The peak of surface plasmon is at 550 nm with a red shift of 30 nm compared with that of Au nanoparticles in water. Monolayers of composite Au/TiO₂ nanoparticles were obtained by dip-coating technique. The XRD pattern of Au/TiO₂ powders resembles a mixture of anatase TiO₂ and gold.     

Effect of deposition parameters on morphology and size of FeCo nanoparticles synthesized by pulsed laser ablation deposition

The experimental parameters that control the surface morphology and size of iron cobalt nanoparticles synthesized at room temperature by pulsed laser ablation deposition (PLAD) technique have been systematically investigated. The nanoparticle synthesis has been achieved at higher operating gas pressures of argon. It was found that nanoparticles upon deposition formed small clusters, the size of which increases with decreasing pressure, increasing laser-energy density, and decreasing target-to-substrate distance. This trend could be attributed to change in the kinetic energy of deposited nanoparticles with varying argon pressure, laser-energy, and target-to-substrate distance. The nanoparticles size and size distribution showed strong dependence on argon pressure and weak dependence on laser-energy density and target-to-substrate distance.     

Structural characterization of AlN films synthesized by pulsed laser deposition

We obtained AlN thin films by pulsed laser deposition (PLD) from a polycrystalline AlN target using a pulsed KrF* excimer laser source (248 nm, 25 ns, intensity of ∼4 × 10⁸ W/cm², repetition rate 3 Hz, 10 J/cm² laser fluence). The target-Si substrate distance was 5 cm. Films were grown either in vacuum (10⁻⁴ Pa residual pressure) or in nitrogen at a dynamic pressure of 0.1 and 10 Pa, using a total of 20,000 subsequent pulses. The films structure was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and spectral ellipsometry (SE). Our TEM and XRD studies showed a strong dependence of the film structure on the nitrogen content in the ambient gas. The films deposited in vacuum exhibited a high quality polycrystalline structure with a hexagonal phase. The crystallite growth proceeds along the c-axis, perpendicular to the substrate surface, resulting in a columnar and strongly textured structure. The films grown at low nitrogen pressure (0.1 Pa) were amorphous as seen by TEM and XRD, but SE data analysis revealed ∼1.7 vol.% crystallites embedded in the amorphous AlN matrix. Increasing the nitrogen pressure to 10 Pa promotes the formation of cubic (≤10 nm) crystallites as seen by TEM but their density was still low to be detected by XRD. SE data analysis confirmed the results obtained from the TEM and XRD observations.     

Ultra-fast laser ablation and deposition of TiO2

In this work we report on the properties of the ablation plume and the characteristics of the films produced by ultra-fast pulsed laser deposition (PLD) of TiO₂ in vacuum. Ablation was induced by using pulses with a duration of ≈300 fs at 527 nm. We discuss both the composition and the expansion dynamics of the TiO₂ plasma plume, measured by exploiting time- and space-resolved emission spectroscopy and gated imaging. The properties of the TiO₂ nanoparticles and nanoparticle-assembled films were characterized using different techniques, i.e. environmental scanning electron microscopy (ESEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). It is suggested that most of the material decomposes in the form of nanoparticles.     

Production and characterization of boron nanoparticles synthesized with a thermal plasma system

A new method for the production of boron nanoparticles is described. Boron trichloride is dissociated through injection into thermal plasma followed by a nucleation process producing boron nanoparticles. The ambient oxidation of the as-produced nanoparticles is also investigated. The nanoparticles were characterized with scanning transmission electron microscopy, electron energy loss spectroscopy, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy to investigate their purity and stability under ambient conditions.     

Sonochemically synthesized MnO2 nanoparticles as electrode material for supercapacitors

In this study, manganese oxide (MnO₂) nanoparticles were synthesized by sonochemical reduction of KMnO₄ using polyethylene glycol (PEG) as a reducing agent as well as structure directing agent under room temperature in short duration of time and characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Transmission electron microscopy (TEM) and Brunauer–Emmett–Teller (BET) analysis. A supercapacitor device constructed using the ultrasonically-synthesized MnO₂ nanoparticles showed maximum specific capacitance (SC) of 282 Fg⁻¹ in the presence of 1 M Ca(NO₃)₂ as an electrolyte at a current density of 0.5 mA cm⁻² in the potential range from 0.0 to 1.0 V and about 78% of specific capacitance was retained even after 1000 cycles indicating its high electrochemical stability.     

Effects of target-substrate geometry and ambient gas pressure on FePt nanoparticles synthesized by pulsed laser deposition

FePt nanoparticles, in the forms of nanoparticle agglomerates and floccules-like nanoparticle networks, can be synthesized by pulsed laser deposition (PLD) at different ambient gas pressures. Backward plume deposition (BPD), as special target-substrate geometry, can achieve higher uniformity in terms of agglomerate size and size distribution, compared to conventional PLD. Both as-deposited FePt nanoparticles exhibit low K_u fcc phase and post-annealing at 600 °C is required for the phase transition to high K_u fct phase. FePt nanoparticle agglomerates deposited by BPD were found to have better fct phase crystallinity after annealing, which may be caused by the higher kinetic energy of backward moving ablated species due to shorter travel distance.     

Field emission studies of silver nanoparticles synthesized by electron cyclotron resonance plasma

Field emission has been studied for silver nanoparticles (25-200 nm), deposited within a cylindrical silver target in an electron cyclotron resonance (ECR) plasma. Particle size distribution was controlled by optimum biasing voltages between the chamber and the target. Presence of non-oxidized silver was confirmed from the X-Ray diffraction analysis; however, thin protective layer of oxide was identified from the selective area electron diffraction pattern obtained with transmission electron microscopy. The silver nanoparticles were seen to exhibit hilly pointed like structures when viewed under the atomic force microscopy (AFM). The emissive properties of these particles were investigated by field emission microscopy. It is found that this technique of deposition is ideal for formation of nanoparticles films on different substrate geometries with size controllability as well as its application to emission devices.     

Luminescence characteristics of cobalt doped TiO2 nanoparticles

TiO₂ nanoparticles doped with two different concentrations of Cobalt, 0.02 and 0.04 mol, are prepared by sol–gel method. The crystalline phase of the doped and undoped nanoparticles and particle sizes are observed with X-ray diffraction and transmission electron microscope. FTIR confirms the bonding interaction of Co²⁺ in TiO₂ lattice framework. The UV absorption spectra of the doped material shows two absorption peaks in the visible region related to d–d electronic transitions of Co²⁺ in TiO₂ lattice. Compared to undoped TiO₂ nanoparticles, the cobalt doped samples show a red shift in the band gap. Steady state photoluminescence spectra give emission peaks related to oxygen defects. The decrease in the intensity ratio of UV/visible emission peaks confirms distortion of structural regularity and formation of defects after doping. The intensity ratio of different visible emission peaks is nearly same for undoped and 0.02 Co²⁺. However, this ratio decreases profoundly at 0.04 Co²⁺, due to concentration quenching effect. Photoluminescence excitation spectra, recorded at 598 nm emission wavelength, give different excitation peaks associated with oxygen vacancies and Co²⁺. Time resolved photoluminescence spectra give longer decay time for doped samples, indicating longer relaxation of conduction band electrons on the defect and on dopant sites.     

Atomic layer deposition of TiO2 and Al‐doped TiO2 films on Ir substrates for ultralow leakage currents

TiO₂ and Al‐doped TiO₂ (ATO) films were grown on Ir substrates by atomic layer deposition using O₃ as the oxygen source. With increasing O₃ feeding time, the crystalline structure of the TiO₂ films was transformed from anatase to rutile. Above an O₃ feeding time of 35 s, the films crystallized as only rutile due to the formation of IrO₂ layer at the interface. The TiO₂ and ATO films showed higher dielectric constants of 78 and 51, respectively. The films on Ir showed superior leakage properties compared to the films on Ru due to the high work‐function of Ir. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of permalloy nanostructured films by deposition of laser ablated nanoparticles

A permalloy (Ni₈₁Fe₁₉; at%) microparticle (MP) aerosol was ablated to produce a nanoparticle (NP) aerosol that was then impacted at high velocity onto a substrate to produce porous thick films. The structure of the NPs was analyzed by transmission electron microscopy and the morphologies of the NPs and the nanostructured films were studied using high-resolution transmission electron microscopy and scanning electron microscopy. These analyses showed that the original composition and structure of the MPs were preserved in the NPs and films. The majority of NPs that were produced ranged in size between 2 and 15 nm with some larger particles present. Magnetization-temperature curves showed that the films consisted of a mixture of small superparamagnetic NPs and larger ferromagnetic NPs. A high saturation magnetization of 62.3 emu/g at 300 K was retained in the films indicating that they remained free of significant oxidation.     

Parametric studies on iron-carbon composite nanoparticles synthesized by laser pyrolysis for increased passivation and high iron content

Iron/iron carbide core and carbon shell nanoparticles with improved magnetic properties were successfully synthesized by laser pyrolysis. As iron and carbon precursors, iron pentacarbonyl and pure or argon-diluted acetylene/ethylene mixtures, respectively, were used. The aim of the present optimization is the improvement of the magnetic properties of the nanomaterials by the increase of the iron percent in powders simultaneously to the maintaining of the protective character of the carbon coverage of nanoparticles. The chemical content and the crystalline structure were monitored by EDX, XRD and TEM techniques. In the first study, the content of acetylene as carbon source was diminished from 75% to 0%. Consequently the percent iron increased from 10 at.% to 28 at.% while oxygen remained relatively constant (around 5 at.%). In the second step, only diluted ethylene was used (maximum 87.5 vol.% Ar). In this case, an increase of iron to 46 at.% is observed. An optimum 50% carbon source dilution was found. Above this value, the carbon content increases and below it, superficial oxidation increases through the diminishing of the carbon shell. The magnetic properties and the Fe phase composition of the Fe-C samples were analyzed by temperature dependent Mössbauer spectroscopy.     

Generation and characterization of stable, highly concentrated titanium dioxide nanoparticle aerosols for rodent inhalation studies

The intensive use of nano-sized titanium dioxide (TiO₂) particles in many different applications necessitates studies on their risk assessment as there are still open questions on their safe handling and utilization. For reliable risk assessment, the interaction of TiO₂ nanoparticles (NP) with biological systems ideally needs to be investigated using physico-chemically uniform and well-characterized NP. In this article, we describe the reproducible production of TiO₂ NP aerosols using spark ignition technology. Because currently no data are available on inhaled NP in the 10?C50 nm diameter range, the emphasis was to generate NP as small as 20 nm for inhalation studies in rodents. For anticipated in vivo dosimetry analyses, TiO₂ NP were radiolabeled with ⁴⁸V by proton irradiation of the titanium electrodes of the spark generator. The dissolution rate of the ⁴⁸V label was about 1% within the first day. The highly concentrated, polydisperse TiO₂ NP aerosol (3?C6 × 10⁶ cm^?3) proved to be constant over several hours in terms of its count median mobility diameter, its geometric standard deviation, and number concentration. Extensive characterization of NP chemical composition, physical structure, morphology, and specific surface area was performed. The originally generated amorphous TiO₂ NP were converted into crystalline anatase TiO₂ NP by thermal annealing at 950 °C. Both crystalline and amorphous 20-nm TiO₂ NP were chain agglomerated/aggregated, consisting of primary particles in the range of 5 nm. Disintegration of the deposited TiO₂ NP in lung tissue was not detectable within 24 h.     

Structural characterization and magnetic properties of superparamagnetic zinc ferrite nanoparticles synthesized by the coprecipitation method

Single phase zinc ferrite (ZnFe₂O₄) nanoparticles have been prepared by the coprecipitation method without any subsequent calcination. The effects of precipitation temperature in the range 20–80 °C on the structural and the magnetic properties of zinc ferrite nanoparticles were investigated. The crystallite size, microstructure and magnetic properties of the prepared nanoparticles were studied using X-ray diffraction (XRD), Fourier transmission infrared spectrum, transmission electron microscope (TEM), energy dispersive X-ray spectrometer and vibrating sample magnetometer. The XRD results showed that the coprecipitated nanoparticles were single phase zinc ferrite with mixture of normal and inverse spinel structures. Furthermore, ZnFe₂O₄ nanoparticles have the crystallite size in the range 5–10 nm, as confirmed by TEM. The magnetic measurements exhibited that the zinc ferrite nanoparticles synthesized at 40 °C were superparamagnetic with the maximum magnetization of 7.3 emu/g at 10 kOe.     

A review of characterization and physical property studies of metallic nanoparticles

In this survey, the characterization of metallic nanoparticles prepared by various methods and the physical properties including the theory and measurements of linear and nonlinear optics, electric and magnetic properties are reviewed. Technical results involving linear optical absorption, optical second harmonic generation, temperature dependence of resistivity, electron paramagnetic resonance and magnetic susceptibility measurements were portrayed. A number of fascinating and provocative results have been developed that lead our perspective understanding of quantum size confinements.     

Preparation and characterization of polyethylene/TiO2 nanocomposites

The rheological behaviour, dispersion, crystallization behavior, mechanical properties, fracture surface morphology of polyethylene (PE)/TiO₂ nanocomposites prepared by melt compounding were investigated using rheometer, energy dispersive X-ray spectrometer (EDX), polarized microscopy, impact tester, universal testing machine and field-emission scanning electron microscopy (FE-SEM). The rheological analysis indicated a fine dispersion of TiO₂ during the melt compounding. The large scaled surface dispersion of TiO₂ nanoparticles was revealed by the EDX composition distribution maps. The introduction of 2.0 wt% TiO₂ in composites improved the mechanical properties significantly compared to neat PE, and resulted in 45% increase in notched impact strength. Moreover, the further analysis and discussion showed the mechanical properties of the composites were controlled by the dispersion conditions of TiO₂ and its nucleating effect on PE crystallization.