Optical properties of silicon nanoparticles synthesized via electrical spark discharge in water

In this paper, we report a simple and low-cost technique for fabrication of silicon nanoparticles via electrical spark discharge between two plane silicon electrodes immersed in deionized water (DI). The pulsed spark discharge with the peak current of 60 A and a duration of a single discharge pulse of 60 μs was used in our experiment. The structure, morphology, and average size of the resulting nanoparticles were characterized by means of X-Ray Diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). TEM images illustrated nearly spherical and isolated Si nanoparticles with diameters in the 3–8 nm range. The Raman peaks of the samples were shifted to the lower wave numbers in comparison to this of bulk crystalline silicon indicating the existence of tiny particles. The optical absorption spectrum of the nanoparticles was measured in the violet–visible (UV–Vis) spectral region. By measuring of the band gap we could estimate the average size of the prepared particles. The silicon nanoparticles synthesized exhibited a photoluminescence (PL) band in the violet-blue region with a double peak at around 417 and 439 nm. It can be attributed to oxide-related defects on the surface of silicon nanoparticles, which can act as the radiative centers for the electron-hole pair recombination.     

Synthesis of composite gold/tin-oxide nanoparticles by nano-soldering

Composite Au–SnO₂ nanoparticles (NPs) are synthesized by nano-soldering of pure Au and SnO₂ NPs. The multi-step process involves synthesis of pure Au and SnO₂ NPs separately by nanosecond pulse laser ablation of pure gold and pure tin targets in deionized water and post-ablation laser heating of mixed solution of Au colloidal and SnO₂ colloidal to form nanocomposite. Transmission Electron Microscopy (TEM) and High-Resolution Transmission Electron Microscopy (HRTEM) were used to study the effect of laser irradiation time on morphology of the composite Au–SnO₂ NPs. The spherical particles of 4 nm mean size were obtained for 5 min of post-laser heating. Increased mean size and elongated particles were observed on further laser heating. UV–vis spectra of Au–SnO₂ nanocomposites show red shift in the plasmon resonance absorption peak and line shape broadening with respect to pure Au NPs. The negative binding energy shift of Au 4f_7/2 peak observed in X-ray Photoelectron Spectra (XPS) indicates charge transfer in the nano-soldered Au–SnO₂ between gold and tin oxide and formation of soldered nanocomposite.     

Influence of Liquid Medium on Optical Characteristics of the Si Nanoparticles Prepared by Submerged Electrical Spark Discharge

We have measured the size, structure, and optical properties for two sets of nanoparticles synthesized via electrical-spark discharge between two plane silicon electrodes immersed in deionized water (DI) and 97 % ethanol. The nanoparticles were characterized by X-ray diffraction (XRD), ultraviolet (UV)-visible absorption spectrometry, Raman spectrometry, transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FTIR). The size and optical features of the nanoparticles were studied as functions of nature of the liquid. Nearly spherical, single-crystal, and morphologically similar Si nanoparticles with diameters in the 3–8 and 6–13 nm ranges were formed in the colloidal solutions of water and ethanol, with estimated indirect bandgaps of approximately 1.5 and 1.3 eV, respectively. In both cases, the Raman peaks were blue shifted with respect to those of bulk silicon, a result consistent with the small diameters of the particles. The silicon nanoparticles synthesized in water exhibited strong emission in the violet-blue range, with a double peak near 417 and 439 nm. For those synthesized in ethanol, blue-green emission centered at 463 nm was detected.     

Fabrication of gold nanoparticles in water by laser ablation technique and their characterization

A colloidal solution of gold nanoparticles in deionized nanopure water was produced by laser ablation technique without the use of any chemical/surfactant. Spectral characterization and morphological studies of these nanoparticles were carried out by UV-Vis Spectroscopy and Scanning Electron Microscopy, respectively. A number of variables of the ablating laser pulse have been used to control the size of the fabricated nanoparticles. Excellent correlation between ablating laser pulse parameter and optical and morphological parameters of the gold colloids were obtained. The peak of the extinction spectra shows a monotonic blue shift for laser fluence of 410 J/cm² and above. Below this the extinction peak remains fairly constant in wavelength. Blue shifts of the extinction spectra were also observed with increasing re-ablation time of previously ablated gold colloids. Possible explanations of all these observations are discussed.     

Pulsed-laser generation of gold nanoparticles with on-line surface plasmon resonance detection

Size of nanoparticles is an important parameter for their applications. The real-time monitoring is required for reliable and reproducible production of nanoparticles with controllable size. We present results of our research on development of the system for the online nanoparticle characterization during their production by a laser. The laser ablation chamber which allows measurements of surface plasmon resonance spectra during the nanoparticle generation process has been designed and fabricated. The online characterization system was tested by producing and modification of gold nanoparticles. Nanoparticles were generated by nanosecond-laser (wavelength 1064 nm) ablation of gold target in deionized water, and optimal conditions for the highest nanoparticle productivity were estimated. The mean diameter of nanoparticles was determined using their absorption spectra measured in the real-time during the ablation experiments and from the TEM images analysis, and it varied from 20 to 45 nm. The mismatch between nanoparticle diameters, estimated using these two methods, is due to the polydispersity of the generated nanoparticles. The further experiments of laser-induced modification of colloidal gold nanoparticles were carried out using second harmonic (wavelength 532 nm) of nanosecond Nd:YAG laser and alteration in nanoparticle size were acquired by the online measurement system.     

Polylactic acid (PLA)/Silver-NP/VitaminE bionanocomposite electrospun nanofibers with antibacterial and antioxidant activity

The antibacterial property of silver nanoparticles (Ag-NPs) and the antioxidant activity of Vitamin E have been combined by incorporation of these two active components within polylactic acid (PLA) nanofibers via electrospinning (PLA/Ag-NP/VitaminE nanofibers). The morphological and structural characterizations of PLA/Ag-NP/VitaminE nanofibers were performed by Scanning Electron Microscopy (SEM), Transmission Electron Microscopy and X-ray diffraction. The average fiber diameter was 140 ± 60 nm, and the size of the Ag-NP was 2.7 ± 1.5 nm. PLA/Ag-NP/VitaminE nanofibers inhibited growth of Escherichia coli, Listeria monocytogenes and Salmonella typhymurium up to 100 %. The amount of released Ag ions from the nanofibers immersed in aqueous solution was determined by Inductively Coupled Plasma Mass Spectrometry, and it has been observed that the release of Ag ions was kept approximately constant after 10 days of immersion. The antioxidant activity of PLA/Ag-NP/VitaminE nanofibers was evaluated according to DPPH (2,2-diphenyl-1-picrylhydrazyl) method and determined as 94 %. The results of the tests on fresh apple and apple juice indicated that the PLA/Ag/VitaminE nanofiber membrane actively reduced the polyphenol oxidase activity. The multifunctional electrospun PLA nanofibers incorporating Ag-NP and Vitamin E may be quite applicable in food packaging due to the extremely large surface area of nanofibers along with antibacterial and antioxidant activities. These materials could find application in food industry as a potential preservative packaging for fruits and juices.     

Investigation of size distribution of silver nanoparticles

In this work, we present a physical methodology of preparing silver nanoparticles suspended in the deionized water. For this purpose, we apply the DC spark method and present the size distribution (by Zetasizer) and optical properties (by UV/VIS) of the nanoparticles in two different voltages. The obtained results using the DC spark method show that the fabrication of silver nanoparticles in deionized water without any surfactants and stabilizers is relatively cheap and pollution free. Using the method, we could prepare the silver nanoparticles smaller than 5 nm.     

Two-step femtosecond laser ablation-based method for the synthesis of stable and ultra-pure gold nanoparticles in water

A two-step laser-assisted method for the synthesis of small and low-dispersed colloidal gold nanoparticles in deionized water is reported. As the first step, laser ablation from a gold target is used to fabricate relatively large (few tens of nanometers) and size-dispersed colloids. As the second step, self-modification of the femtosecond laser pulse into a white-light supercontinuum is used to perform the secondary ablation of colloids. We show that the latter treatment leads to a drastic reduction of both the mean nanoparticles size and size dispersion as well as to the enhancement of the solution stability. Being prepared in pure deionized water, the colloidal nanoparticles are stable and free of any impurities, making them unique for surface enhanced Raman scattering (SERS) and bio-imaging in vivo applications. PACS 81.05.-t; 82.70.Dd     

Advantages and limitations of OM, SEM, TEM and AFM in the study of ancient decorated pottery

This paper presents results from the study of two fragments of pre-Hispanic pottery, decorated with red pigment, using Optical Microscopy (OM), Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM), Atomic Force Microscopy (AFM) and Magnetic Force Microscopy (MFM). Capabilities and limitations of these techniques in the analysis of archaeological material are highlighted with special emphasis on TEM, AFM and MFM due to their contribution in the study of the pigment layer at micro and nano scale. The analyzed samples come from the archaeological sites of El Tajin and Xochicalco, both in Mexico. Results of conventional TEM and HRTEM analysis of the red pigment showed nanometric Fe₂O₃ particles in both samples but different particle shape and size distributions: specimen from El Tajin presented irregular particles between 50–100 nm while that from Xochicalco exhibited semispherical shapes in the 3–25 nm range. AFM images showed the topography of the pigments, which are related to the texture of their surface and thus to the production process. Finally, MFM showed different contrast regions suggesting the presence of ferromagnetic elements forming clusters and domain orientations on the color layer.     

Synthesis and electrochemical characterization of graphene nanoflakes and LiFe<Subscript>0.97</Subscript>Ni<Subscript>0.03</Subscript>PO<Subscript>4</Subscript>/C for lithium-ion battery

The graphene nanoflakes and olivine-type LiFe_0.97Ni_0.03PO₄/C (LFNP3/C) samples have been synthesized as anode and cathode materials, respectively. Physicochemical characterization of the graphene nanoflakes and LFNP3/C material were studied using X-ray diffraction (XRD) and scanning electron microscope (SEM). The XRD patterns reveal the formation of the pure phase of both the synthesized samples. SEM micrographs disclose the formation of spherically shaped nanosized particles for LFNP3/C while graphene shows flake-type morphology. CR2032 half and full coin cells were assembled for electrochemical testing of the synthesized samples. Cyclic voltammetry (CV) results indicate that the graphene-based half-cells, i.e., GN1H and GN2H, possess reduction peak/plateau around 0.17 V while LFNP3/C cathode shows discharging voltage plateau at 3.4 V vs. Li/Li⁺. The discharge capacities were found to be 700, 900, and 153 mAhg^?1 for GN1H, GN2H, and LFNP3/C half-cells vs. Li/Li⁺, respectively. Among full cells, LFPGN1F with γ = 0.75 (mass/capacity balancing factor) shows better charging/discharging profile at each C-rate as compared to LFPGN2F with γ = 0.55. LFPGN1F delivered an initial discharge capacity of around 154 mAhg^?1 at 0.1C and even at a high discharge rate of 1C, it retained ~97% of the discharge capacity as compared to the initial cycle at the same rate.     

Composition distributions in FePt(Au) nanoparticles

Ternary alloy FePt(Au) nanoparticles were prepared by the co-reduction of platinum(II) acetylacetonate and gold(III) acetate and the thermal decomposition of iron pentacarbonyl in hot phenyl ether in the presence of oleic acid and oleylamine ligands. This gave spherical particles with an average diameter of 4.4 nm with a range of diameters from approximately 1.6–9 nm. The as-synthesized particles had a solid solution, face-centered-cubic structure. Though the average composition of the particles was Fe₄₄Pt₄₅Au₁₁, individual particle analysis by Scanning Transmission Electron Microscopy–X-ray Energy Dispersive Spectroscopy showed a broad distribution in composition. In general, smaller-sized particles tended to have a lower amount of Au as compared to larger-sized particles. As the Au content increased, the ratio of Fe/Pt widened.     

One-step,template-free hydrothermal synthesis of CuO tetrapods

The present investigation reports one-step template-free hydrothermal synthesis of CuO tetrapods (CuO-T) and its characterization. The CuO tetrapods have been prepared in moderate condition without using any surfactant. The prepared sample was characterized by powder X-ray diffraction (PXRD), Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy, UV–vis–NIR (DRS) spectroscopy and Photoluminescence (PL) spectroscopy. The X-ray diffraction and Fourier transform infrared spectrum analysis confirm clearly the formation of a pure phase high-quality CuO with monoclinic crystal structure. X-ray peak broadening analysis was used to evaluate the average crystallite size (∼30 nm) and lattice strain by the Williamson–Hall (W–H) method. Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) result reveals that the particles are tetrapods in shape with an average length ∼50 nm. Additionally the optical properties were investigated by using UV–vis reflectance spectra with considerable blue-shift in the optical band gap (Eg = 1.45 eV) due to quantum confinement effect. Photoluminescence (PL) spectrum showed both UV as well as visible emission peaks indicating their good optical properties.     

A novel approach to metal and metal oxide nanoparticle synthesis: the oil-in-water microemulsion reaction method

A novel and straightforward approach, based on oil-in-water (o/w) microemulsions, was developed for the synthesis of inorganic nanoparticles at ambient conditions. It implies the use of organometallic precursors dissolved in nanometre-scale oil droplets of o/w microemulsions. Addition of reducing or oxidizing/precipitating agents results in the formation of metallic or metal oxide nanoparticles, respectively. Nonionic o/w microemulsion systems were chosen, and several key compositions were selected for nanoparticle synthesis at 25 °C. High Resolution Electron Microscopy revealed that small nanoparticles of metals (Pt, Pd and Rh) and nanocrystalline metal oxide (cerium (IV) oxide with cubic type crystalline structure confirmed by XRD), of less than 7 nm can be obtained in mild conditions.     

Synthesis of silver nanoparticles and antimony oxide nanocrystals by pulsed laser ablation in liquid media

Pulsed laser ablation in liquid media (PLALM) is a prominent technique for the controlled fabrication of nanomaterials via rapid reactive quenching of ablated species at the interface between the plasma and liquid. Results on nanoparticles and nanocrystals formed by PLALM of silver (Ag) and antimony (Sb) solid targets in different liquid environments (Sodium Dodecyl Sulfate, distilled water) are presented. These experiments were done by irradiating solid targets of Ag and Sb with a nanosecond pulsed Nd:YAG laser output of wavelength 532 nm. Nanoparticles of silver and nanocrystals of antimony oxide (Sb₂O₃) obtained were characterized using UV-Vis spectrometry, Scanning Electron Microscopy (SEM), transmission electron microscopy (TEM), X-ray Energy Dispersion Analysis (EDAX) and X-ray diffractometry (XRD). The morphology of nanomaterials formed is studied as a function of surfactant environment. The silver nanoparticles obtained were spherical of size in the order of 10–35 nm in solution of SDS having different concentrations. In case of the Sb target, ablation was performed in two different molarities of SDS solution and distilled water. Nanocrystals of Sb₂O₃ in powder form having cubic and orthorhombic phases were formed in SDS solution and as fibers of nanocrystals of cubic Sb₂O₃ in distilled water.     

From polymer films to organic nanoparticles suspensions by means of excimer laser ablation in water

This study highlights the preparation of organic nanoparticles (NP) by laser ablation (LA) of polymeric materials in water. Experiments focused on poly(ethylene terephtalate) (PET) were carried out with the KrF laser pulse (248 nm). Size distribution and concentration of nanoparticles were deduced from suspensions turbidity measurements with the aid of Mie model, by Atomic Force Microscopy (AFM) on the basis of a statistical study and Scanning Electron Microscopy (SEM). The obtained results show that assemblies of spherical NP with a mean diameter 50 nm were synthesised. Composition and surface chemistry of NP were investigated using the Confocal Micro-Raman Spectroscopy (CMRS) and X-ray Photoelectron Spectroscopy (XPS). It indicates that NP are graphitic carbon rich and have a polymeric structure like polyacetylene. The possible mechanisms responsible of NP synthesis by under water LA of polymers was briefly discussed by investigating other polymers targets.     

Preparation and characterization of SnO2 nanoparticles using high power pulsed laser

Tin dioxide (SnO₂) nanoparticles having 3 nm size were synthesized by irradiating pure tin metal using high power Nd:YAG laser in deionized water. Formation of nano-SnO₂ crystallites was confirmed by X-ray diffraction (XRD) and AFM study. UV-vis absorption spectral studies showed a peak at 240 nm. FTIR spectrum showed a band in the range of 400-700 cm⁻¹ which was assigned to Sn-O antisymmetric vibrations. Photoluminescence spectrum of synthesized SnO₂ nanoparticles showed peak corresponding to 3.175, 2.901 and 2.613 eV respectively.     

Laser-assisted shape selective fragmentation of nanoparticles

Experimental results are presented on laser-assisted fragmentation of gold-containing nanoparticles suspended in liquids (either ethanol or water). Two kinds of nanoparticles are considered: (i) elongated Au nanorods synthesized by laser ablation of a gold target immersed in liquid phase; (ii) gold-covered NiCo nanorods with high aspect ratio (θ ∼ 10) synthesized by wet chemistry processes. The shape selectivity induced by laser fragmentation of these nanorods is gained via tuning the wavelength of laser radiation into different parts of the spectrum of their plasmon resonance corresponding to different aspect ratios θ. Fragmentation is performed using three laser wavelengths, involving a Cu vapour laser (510 and 578 nm) and a Nd:YAG (1064 nm). Nanoparticles are characterized by UV-vis spectrometry, Transmission Electron Microscopy (TEM). The effect of laser pulse duration (nanosecond against picosecond range) is also studied in the case of fragmentation with an IR laser radiation.     

Synthesis of ZnO nanowires on aluminum flake by aqueous method

ZnO nanowires are grown on aluminum flake at low temperature by using a simple aqueous solution method. X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscope (TEM) are applied to determine the as-grown ZnO nanowires morphology and crystal structures. The results show that the ZnO nanowires have wurtzite structure, and the diameter and length of the nanowire are 30 nm and more than 1.5 μm, respectively. Photoluminescence spectroscopy (PL) and Raman spectrum reveal the nanowires have good optical properties with low tensile stress. Meanwhile, photoelectrochemical cell (PEC) study verifies that ZnO nanowires as photoanodes are relatively stable in the photo-oxidation process, which could be a promising technique for practical applications.     

Synthesis and characterization of S-Au interaction in gold nanoparticle bound polymeric beads

A detailed X-ray Absorption Spectroscopic examination of S-Au interaction in gold nanoparticle bound to Polystyrene-Divinyl Benzene (PS-DVB) micro beads was carried out. Gold nanoparticles were bound to the surface of the commercially available PS-DVB beads using a simple one step procedure. Influence of polystyrene backbone on the electronic structure of the gold nanoparticles was observed through X-ray Absorption Near Edge Structure (XANES) spectra of Au at L III edge. An additional structure in the white line of the S K-edge XANES spectrum confirmed the presence of S-Au bonding. Transmission Electron Microscopy (TEM) studies coupled with Selected Area Electron Diffraction Pattern and X-ray Diffraction studies revealed the morphology of the Au nanoparticles bound to the micro beads.     

Synthesis and characterization of poly(N-methylpyrrole)/TiO2 composites on steel

Poly(N-methyl pyrrole) coating was successfully electrodeposited on steel substrates in mixed electrolytes of dodecyl benzene sulphonic acid (DBSA) with oxalic acid in the absence and the presence of TiO₂ nanoparticles (NPs). The morphology and compositions were characterized by Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform Infrared Spectroscopy (FTIR), Energy-Dispersive X-ray spectroscopy (EDX). X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) were used to calculate the size of nanoparticles. Electrode/polymer/electrolyte system was studied by Electrochemical Impedance Spectroscopy (EIS). The FESEM micrographs suggest that the incorporation of TiO₂ nanoparticles affects the morphology of the film significantly and makes the TiO₂ to be loosely piled up with PMPy. The results of EIS showed that synthesized PMPy in the presence of TiO₂ NPs increases and decreases the R_po and C_c of the coating respectively. The increase of the area of synthesized PMPy in the presence of nanoparticles can increase its ability to interact with the ions liberated during the corrosion reaction of steel in NaCl solution.