Size-controlled hydrothermal synthesis of monodispersed BaZrO3 sphere particles by seeding

Monodispersed barium zirconate (BaZrO₃) fine particles with a spherical shape have been synthesized by hydrothermal reactions using barium hydroxide and a Zr-triethanolamine (TEOA) complex. The particle mean diameter was gradually controlled in a range from 0.20 μm to 3.5 μm by change in the added amount of seed nanoparticles. The mechanistic characterization of the seed-mediated BaZrO₃ sphere synthesis revealed that the particle growth obeyed a simple seed growth mechanism. In the present system, utilization of the Zr-TEOA complex played an important rule to prevent uncontrollable nucleation to form the uniform BaZrO₃ fine particles with narrow size distributions.     

Influence of processing method on the properties of hydroxyapatite nanoparticles in the presence of different citrate ion concentrations

The objective of this study was to investigate the effect of processing methods on the formation of ultra fine hydroxyapatite (HAp) nanoparticles in the presence of citrate ions and analyze their various physical properties. The addition of the citrate ions was found to reduce the size and prevent the agglomeration of HAp particles dramatically in the high gravity (HG) method compared to precipitation method. In precipitation method, the particle size reduced from 300 ± 70 nm to 90 ± 20 nm with the addition of citrate ions. In high gravity method, the particle size decreased more significantly from 80 ± 10 nm to 13 ± 5 nm with the addition of citrate ions. Furthermore, more uniform size distribution of nanoparticles was achieved in high gravity method. X-ray diffraction of nanoparticles prepared in both method exhibited slight shift of peaks to the higher angle with the addition of citric acid, indicating the incorporation of carbonate (CO₃) content in the HAp nanoparticles irrespective of the particle size. The mechanical properties of HWMPE matrix composite reinforced with nanoparticles was examined and this nanocomposite with nanoparticles prepared in high gravity method with the addition of citrate ions showed increased mechanical strength due to the considerable reduction in the particle size and higher uniformity of the particles. In vitro cellular analyses of the nanoparticle prepared in high gravity with the addition of citrate ions also displayed the most pronounced spreading of cell growth.     

Dynamic light scattering and UV–vis spectroscopy of gold nanoparticles solution

Gold nanoparticles solution prepared in water by laser ablation at 1064 nm of a gold metal plate was characterized by dynamic light scattering and UV–vis spectroscopy. Polarized dynamic scattering allows the measurement of translational diffusivity of Au nanoparticles, while depolarized scattering yields simultaneously the characterization of translational and rotational diffusivities. From these measurements the size and shape of Au nanoparticles are determined. Dynamic light scattering yields an average radius of 32 nm for the spherical nanoparticles in as prepared solution. The same measurements performed in an aged solution reveal the formation of ellipsoidal nanoparticles with minor and major semi-axis of 36 nm and 69 nm, respectively. The measured values allow to fit the UV–vis spectra with the Mie-Gans model and to measure the concentration of Au nanoparticles obtaining a complete characterization of their nanostructure. Dynamic light scattering results a powerful technique to characterize the size and shape of gold nanoparticles.     

Synthesis,structure, and optical properties of Au–TiO2 composite thin films

Titanium dioxide (TiO₂) films with varying concentrations of gold particles were synthesized using pulsed DC magnetron sputtering, with the intent to develop infrared reflecting films for use on cars and planes to reduce solar heat load. Under our deposition conditions, the films are smooth (RMS roughness on the order of 1.0–2.0 nm) and consist of rutile TiO₂ with embedded gold. The average gold particle diameter on the sample surface was found to change from 60 to 200 nm as the volume fraction of gold in the films increased from 1.9 to 4.3% (3.5 to 7.9 mol% Au). The maximum reflectance of these films in the infrared region (800–2500 nm) is > 50%, compared with 30% for pure TiO₂. The Maxwell–Garnett equation does not model the reflectance data very well, due to the relatively large gold particle size. Instead, by assuming that the contribution of gold particles to the reflectance response is proportional to their projected areal fraction in an effective medium approximation, we were able to fit the observed reflectance data quite well.     

Sintering behavior of spherical aggregated nanoparticles prepared by spraying colloidal precursor in a heated flow

The sintering behavior of spherical aggregated nanoparticles prepared by spraying colloidal precursor into a heated flow was investigated both experimentally and theoretically. Spherical micrometer-sized particles consisting of compactly aggregated nanoparticles were formed, due to solvent evaporation and the drying process of the colloidal precursor. The degree of sintering of aggregated nanoparticles depended on the furnace temperature profile, residence time and primary particle size of the aggregated nanoparticles. Spherical monodispersed colloidal silica, in sizes ranging from 22 to 100 nm was selected as the primary particles. The sintering rate increased with temperature and residence time, and decreased with increasing primary particle size. The aggregated nanoparticles sintered completely, resulting in particles with smooth surfaces that were synthesized at 1400 °C, residence time 31.7 s that was obtained by using a carrier gas flow rate of 1.5 L/min and 0.1 M colloidal silica nanoparticles 100 nm in size. An appropriate model of sintering in the system was proposed to explain the shrinkage and the neck growth of the aggregated nanoparticles. The sintering analysis suggested that solid-state volume diffusion suitably described the sintering mechanism of spherical aggregated silica nanoparticles in a heated flow.     

Experimental investigation of the size effects of SiO2 nano-particles on the mechanical properties of binary blended concrete

In the current study, the size effects of SiO₂ nano-particles on compressive, flexural and tensile strength of binary blended concrete were investigated. SiO₂ nano-particles with two different sizes of 15 and 80 nm have been used as a partial cement replacement by 0.5, 1.0, 1.5 and 2.0 wt.%. It was concluded that concrete specimens containing SiO₂ particles with average diameter of 15 nm were harder than those containing 80 nm of SiO₂ particles at the initial days of curing. But this condition was altered at 90 days of curing. Also from the viewpoint of free energy, it can be concluded that the C–S–H gel formation around the particles with average diameter of 15 nm was more at the primary days of curing. This can be as a result of more nucleation sites that causes acceleration in early age strength. On the other hand, the growth probability of C–S–H gel around the 80 nm particles was more at 90 days of moist curing. This is due to the fact that the nucleus of strengthening gel could simply reach to the critical volume of nucleation that causes increase in the strength.     

Characterization of silica-coated Ag nanoparticles synthesized using a water-soluble nanoparticle micelle

This article describes the synthesis of silica-coated Ag nanoparticles using a water-soluble nanoparticle micelle under basic conditions. Monodispersed Ag nanoparticles with a mean particle size of 7 nm were synthesized using AgNO₃ in the presence of ascorbic acid as a reducing agent. The Ag nanoparticles were easily re-dispersed into an aqueous solution by surface adsorption of surfactant molecules, indicating formation of water-soluble nanoparticle micelles. Silica-coated Ag nanoparticles ranging in size from 50 to 100 nm were obtained by controlling the surfactant, Ag nanoparticle and tetraethylortho silicate (TEOS) concentrations. Adsorbed surfactant monolayers on Ag nanoparticles were used as a template for the silica shell because of the hydrophobicity of TEOS. In all cases, the size of the resulting particles increased linearly as these concentrations increased. Based on transmission electron microscopy, all the Ag nanoparticles were completely covered with a silica shell. In most samples, however, Ag nanoparticle size increased from 7 to 50 nm due to evaporation of hexane by heating. Although mean particle size of silica-coated Ag nanoparticles was drastically altered, characteristic absorption peaks were observed at approximately 410 nm.     

Measurement of particle size distribution of silica nanoparticles by interactive force apparatus under an electric field

This paper describes the measurement of particle size distribution of silica nanoparticles by interactive force apparatus (IFA) under an electric field in order to suggest the application of the apparatus to the measurement of particle size distribution. The results were compared with results obtained from size measurement by dynamic light scattering. D₅₀ measured by IFA was closer to the average particle size determined by TEM (5 nm). Also, when compared the results under three different supply voltage, (1) the results at 0.01 and 0.02 V were almost identical while (2) these results were different from the one at 0.04 V. The results indicate that breakage of coagulated particles possibly occur due to electric breakdown. The distribution measured by IFA (D₅₀ = 5–7 nm) was larger than the one measured by DLS (D₅₀ = 1 nm). The electric breakdown was explained by curve fitting of three different particle size distribution functions with particle size distribution obtained from IFA measurement.     

Synthesis of nanocrystalline GaN from Ga2O3 nanoparticles derived from salt-assisted spray pyrolysis

Gallium nitride (GaN) nanoparticles were successfully produced from nano-sized gallium oxide (Ga₂O₃) particles under a flow of ammonia gas. The gallium oxide nanoparticles were prepared by salt-assisted spray pyrolysis (SASP). Highly crystalline Ga₂O₃ nanoparticles with an average diameter of approximately 10 nm were obtained at various temperatures when a flux salt (LiCl, 5 mol/l) was added to the precursor solution. The effects of the crystallinity of the Ga₂O₃ particles and nitridation time on transformation to GaN were characterized using X-ray diffraction and scanning/transmission electron microscopy. Highly crystalline GaN nanoparticles with a mean size of 23.4 nm and a geometric standard deviation of 1.68 nm were obtained when Ga₂O₃ nanoparticles with relatively low crystallinity were used as the starting material. The resulting GaN nanoparticles showed a photoluminescence peak at 364 nm under UV excitation at 254 nm.     

Spectroscopic properties of B2O3–PbO–Bi2O3–GeO2 glass doped with Sm3+ and gold nanoparticles

Heavy metal oxide B₂O₃–PbO–Bi₂O₃–GeO₂ transparent glass doped with Sm³⁺ was synthesized and implanted with Au⁺ using energy of 300 keV and fluence of 1 × 10¹⁶ cm⁻². The annealing of the implanted glass at moderate temperature below the glass transition temperature induced the nucleation of gold nanoparticles, confirmed by the characteristic absorption band in the visible range and by transmission electron microscopy. Using Miés and Doylés theories for the surface plasmon resonance, the average size of the gold nanoparticles was about 4.6 nm, similar to the values observed by transmission electron microscopy. It was also observed the crystallization of a thin layer of the glass at the implanted surface after annealing, detected by X-ray diffraction and scanning electron microscope. Visible and near-infrared emission of Sm³⁺ was enhanced after annealing of the glass implanted with gold. Judd–Ofelt parameters and radiative parameters were calculated for the glass doped with Sm³⁺ with and without gold nanoparticles.     

Synthesis of TbMnO3 nanoparticles via a polyacrylamide gel route

We report here the synthesis of TbMnO₃ nanoparticles via an acrylamide gel route. XRD, TG analysis, DSC analysis, and FTIR spectroscopy are combinatively used to investigate the thermal decomposition process of precursor xerogels and the formation of TbMnO₃ phase. It is demonstrated that high-phase-purity TbMnO₃ nanoparticles can be prepared by using different chelating agents at a sintering temperature of 800 °C. SEM observation and XRD analysis reveal that the particle size and morphology of the products have a dependence on the chelating agent. The particles prepared using citric acid as the chelating agent appear to be regularly spherical in shape and highly uniform in size with a diameter of ～67 nm, while the sample prepared by using the chelating agent EDTA mainly consists of sphere-, ellipsoid-, and rod-like particles and exhibits a relatively broad particle size distribution with an average particle size centered around 115 nm. The use of a combination of citric acid and EDTA generally results in sphere- and ellipsoid-like particles with an average particle size between those of the samples prepared separately by using the two chelating agents.     

Growth of carbon nanofibers catalyzed by silica-coated copper nanoparticles

Silica-coated copper nanoparticles were synthesized by coating copper nanoparticles with a silica shell through microemulsion. The copper nanoparticles are 30–40 nm in diameter and the silica coating is 10 nm in thickness. After coating, copper nanoparticles were encapsulated in a silica matrix. These particles were used as a catalyst for the growth of carbon nanofibers in a tubular furnace. It is found that carbon nanofibers are mirror-symmetric growth and 100 nm in diameter. During growth, the copper nanoparticles moved out of the silica. As the experiment progressed, the interplanar spacing of copper (2 2 0) increased from 0.1288 nm to 0.1306 nm indicating that (2 2 0) plane exhibited high catalytic activity. The out-of-sync growth of different faces provides new evidence for the research of growth mode in carbon nanofibers.     

Synthesis of spherical NiO nanoparticles through a novel biosurfactant mediated emulsion technique

Spherical nickel oxide nanoparticles were synthesized by microemulsion technique using rhamnolipids as the surfactant along with n-heptane and water. Nickel hydroxide (Ni(OH)₂) particles were first formed which were then calcined to obtain nickel oxide (NiO) particles. Scanning Electron Microscopy (SEM) studies revealed that the synthesized nickel hydroxide particles were spherical in shape with stacked lamellar sheets. Nickel hydroxide was converted to nickel oxide by calcinations at 600 °C for 3 h and was confirmed by X-ray Diffraction (XRD) analysis. Transmission Electron Microscopy (TEM) showed that the nickel oxide particles were crystalline and of uniform size. The effect of pH on particle size was investigated and it was found that the particle size decreased from 86 ± 8 nm at pH 11.6 to 47 ± 5 nm at pH 12.5. A novel method using rhamnolipid biosurfactant for microemulsion synthesis has been demonstrated which offers an eco-friendly alternative to conventional microemulsion technique based on organic surfactants.     

Statistical optimization of experimental parameters for synthesis of manganese carbonate and manganese oxide nanoparticles

Taguchi robust design was used for optimization of direct precipitation reaction conditions in order to simple and fast synthesis of manganese carbonate nanoparticles. Manganese carbonate nanoparticles were synthesized in this study by addition of manganese ion solution to the aqueous carbonate reagent. Effects of several reaction variables, such as manganese and carbonate concentrations, flow rate of reagent addition and temperature on particle size of prepared manganese carbonate were investigated. The significance of these parameters in tuning the size of manganese carbonate particles was quantitatively evaluated by analysis of variance. The results showed that manganese concentration and carbonate concentration in the solutions and also flow rate have significant effects in preparation of manganese carbonate nanoparticles. Also, optimum conditions for synthesis of manganese carbonate nanoparticles via precipitation reaction were proposed. Analysis of variance showed that under the optimum condition, the size of manganese carbonate nanoparticles will be about 54 ± 12 nm. In another part of this study, solid state thermal decomposition reaction of precursor was used for preparation of Mn₂O₃ nanoparticles. The results showed that Mn₂O₃ nanoparticles synthesized via thermal decomposition of manganese carbonate nanoparticles have average size of 90 nm.     

Molten-salt decomposition synthesis of SnO2 nanoparticles as anode materials for lithium ion batteries

SnO₂ nanoparticles were synthesized by a simple, easily scaled-up molten-salt decomposition method with SnSO₄ as the molten salt and the reactive phase. During the synthesis process, the undecomposed molten SnSO₄ makes it possible to obtain SnO₂ nanoparticles by serving as the dispersion medium and keeping the particles from aggregation. The as-prepared SnO₂ had a tetragonal rutile structure with an average particle size of 50 nm. When used as anode materials for lithium ion battery, SnO₂ nanoparticles retained the charge capacity still as high as 402 mAh g^? 1 at a current density of 156 mA g^? 1 after 40 cycles. Moreover, cyclic voltammograms tests showed the formation/deformation of Li₂O was partially reversible.     

Synthesis of nanocrystalline MMoO4 (M = Ni,Zn) phosphors via a citrate complex route assisted by microwave irradiation and their photoluminescence

Nanocrystalline MMoO₄ (M = Ni, Zn) phosphors, which have wolframite-type structure, were successfully synthesized at low temperatures via a modified citrate complex route assisted by microwave irradiation. The citrate complex precursors were heat-treated from 300 to 600 °C for 3 h. Crystallization of the MMoO₄ (M = Ni, Zn) nanocrystallites were detected at 500 °C, and entirely completed at a temperature of 600 °C. The nanoparticles presented primarily dispersed and homogeneous morphology with particle size of 20–40 nm. The nanocrystalline MMoO₄ (M = Ni, Zn) phosphors prepared at 600 °C exhibited broad luminescence in green and blue wavelength region, respectively.     

Synthesis of cobalt boride nanoparticles using RF thermal plasma

Nanosize cobalt boride particles were synthesized from the vapor phase using a 30 kW–4 MHz radio frequency (RF) thermal plasma. Cobalt and boron powder mixtures used as precursors in different composition and feed rate were evaporated immediately in the high temperature plasma and cobalt boride nanoparticles were produced through the quenching process. The X-ray diffractometry (XRD) patterns of cobalt boride nanoparticles prepared from the feed powder ratio of 1:2 and 1:3 for Co:B showed peaks that are associated with the Co₂B and CoB crystal phases of cobalt boride. The XRD analysis revealed that increasing the powder feed rate results in a higher mass fraction and a larger crystalline diameter of cobalt boride nanoparticles. The images obtained by field emission scanning electron microscopy (FE-SEM) revealed that cobalt boride nanoparticles have a spherical morphology. The crystallite size of the particles estimated with XRD was found to be 18–22 nm.     

Synthesis of γ-Al2O3 nanopowders by freeze-drying

This work studies the synthesis of γ-Al₂O₃ nanopowders by a freeze-drying method. Aqueous solutions of Al₂(SO₄)₃·18H₂O were used as precursors to Al concentrations of 0.76, 1.00 and 1.40 M. Homogeneous spherical granules with diameters ranging from 1 to 100 μm have been obtained. These porous granules are constituted by soft agglomerates of nanoparticles with primary particle size lower than 20 nm. The microstructure of the agglomerates largely depends on the freezing kinetics. After drying amorphous aluminium sulphate powder is obtained that decomposes at 825 °C leading to the formation of γ-Al₂O₃. Physicochemical study of the freeze-dried powders is performed through particle size distribution and zeta potential measurements. The characterisation of the powders is evaluated considering the influence of processing parameters such as the salt concentration, the freezing rate and the thermal treatment for the synthesis and the dispersing conditions of the obtained powders. By adjusting the dispersing conditions a minimum particle size <30 nm is measured, thus confirming that granules can be easily dispersed into nanoparticles.     

Synthesis of mesoporous CaCO3 particles by a spray drying method from the stable suspensions achieved in a beads mill

Dispersion of nanoparticles in liquids is an important issue on various applications. CaCO₃ agglomerates were disintegrated into its nanoparticles by a beads mill. The dynamic light scattering (DLS) method showed the size of dispersed particles of 22 nm reduced from the initial size of 130 nm. The effectiveness of smaller beads on the dispersion was explained by their enough impact energy and their high collision frequency. No further grinding of nanoparticles by the beads was explained by the short relaxation time of nanoparticles. The mesoporous CaCO₃ particles were synthesized from the stable suspensions by the spray drying method. As the dispersion air flowrate increased, the particle size decreased due to the smaller droplet size. Non-spherical particles were explained with the velocity difference between the colloidal solution and the dispersion air, with the longer momentum transfer time and with the faster evaporation rate. The pores originated from the spaces between the beads-milled particles, which was also created by the shear force.     

Effect of processing methods on physicochemical properties of titania nanoparticles produced from natural rutile sand

Titania (TiO₂) nanoparticles were produced from natural rutile sand using different approaches such as sol–gel, sonication and spray pyrolysis. The inexpensive titanium sulphate precursor was extracted from rutile sand by employing simple chemical method and used for the production of TiO₂ nanoparticles. Particle size, crystalline structure, surface area, morphology and band gap of the produced nanoparticles are discussed and compared with the different production methods such as sol–gel, sonication and spray pyrolysis. Mean size distribution (d₅₀) of obtained particles is 76 ± 3, 68 ± 3 and 38 ± 3 nm, respectively, for sol–gel, sonication and spray pyrolysis techniques. The band gap (3.168 < 3.215 < 3.240 eV) and surface area (36 < 60 < 103 m² g^?1) of particles are increased with decreasing particle size (76 > 68 > 38 nm), when the process methodology is changed from sol–gel to sonication and sonication to the spray pyrolysis. Among the three methods, spray pyrolysis yields high-surface particles with active semiconductor bandgap energy. The effects of concentration of the precursor, pressure and working temperature are less significant for large-scale production of TiO₂ nanoparticles from natural minerals.