Among the different cancer treatments that are currently used, hyperthermia has a promising potential due to the multiple benefits that are obtained by this technique. In general terms, hyperthermia is a method that takes advantage of the sensitivity of cancer cells to heat, in order to damage or destroy them. Within the different ways of supplying heat to cancer cells and achieve their destruction or damage, the use of magnetic nanoparticles has attracted attention due to the capability of these particles to generate heat under the influence of an external magnetic field. In addition, these nanoparticles have a high surface area and sizes similar or even lower than biological entities, which allow their approaching and interaction with a specific region of interest. The most used magnetic nanoparticles for hyperthermia treatment are those based on iron oxides, mainly magnetite and maghemite, due to their biocompatibility, good magnetic properties and chemical stability. However, in order to fulfill more efficiently the requirements that demand the treatment of magnetic hyperthermia, there have been investigations using ferrites that incorporate different metallic ions, such as Mg, Mn, Co, Ca, Ni, Cu, Li, Gd, etc., in their structure. This paper reports the synthesis of nanosized MgxMn1-xFe2O4 (x = 0.3 and 0.4) ferrites by sol-gel method and their evaluation in terms of heating capability and in vitro hemolysis to determine the potential use of these nanoparticles as thermoseeds for the treatment of cancer by magnetic hyperthermia. It was possible to obtain ferrites with nanometric sizes, a single crystalline phase with an inverse spinel structure and a behavior near to that of superparamagnetic materials. Additionally, at concentrations of 10 mg of magnetic material per mL of water, it was possible to reach a temperature of approximately 45°C, which is within the range of temperatures used for the treatment of hyperthermia. The results of the in vitro hemolysis assay showed that, at the concentrations tested, these nanoparticles are non-hemolytic, as their percentage of hemolysis is close to zero. Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia.
Magnetic spinel ferrites are materials that possess size, magnetic properties and heating ability adequate for their potential use in biomedical applications. The Mn0.5Ga0.5Fe2O4 magnetic nanoparticles (MNPs) were synthesized by sol-gel method using citric acid as chelating agent of metallic precursors. The synthesized samples were identified by X-Ray Diffraction (XRD) as an inverse spinel structure with no secondary phases. Saturation magnetization (Ms) of crystalline powders was 45.9 emu/g, which was higher than those corresponding to GaFe2O4 (14.2 emu/g) and MnFe2O4 (40.2 emu/g) synthesized under similar conditions, while the coercivity field (Hc) was 27.9 Oe. The average particle size was 18 ± 7 nm. The heating ability of the MNPs was enough to increase the surrounding temperature up to 43.5 °C in 7 min when a quantity of 4.5 mg of MNPs per mL of liquid medium was tested. Cytotoxic effect (hemolysis assay) of MNPs was determined and the results showed hemolytic values below 1% in all tested cases. According to the results obtained, these synthesized nanoparticles can be potentially used as thermoseeds for hyperthermia therapy.
Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.
CuAlO2 thin films are prepared on Si or sapphire substrate by sol-gel method using two kinds of sols. One is combination of Cu acetate and Al acetate basic, and the other is Cu nitrate and Al nitrate. In the case of acetate sol, XRD peaks of CuAlO2 observed at annealing temperature of 800-950 ºC on both Si and sapphire substrates. In contrast, in the case of the films prepared using nitrate on Si substrate, XRD peaks of CuAlO2 have been observed only at the annealing temperature of 800-850 ºC. At annealing temperature of 850ºC, peaks of other species have been observed beside the CuAlO2 peaks, then, the CuAlO2 peaks disappeared at annealing temperature of 900 °C with increasing in intensity of the other peaks. Intensity of the other peaks decreased at annealing temperature of 950 ºC with appearance of broad SiO2 peak. In the present, we ascribe these peaks as metal silicide.
Lithium niobate (LiNbO3) nanostructures are prepared on quartz substrate by the sol-gel method. They have been deposited with different molarity concentration and annealed at 500°C. These samples are characterized and analyzed by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and Atomic Force Microscopy (AFM). The measured results showed an importance increasing in molarity concentrations that indicate the structure starts to become crystal, regular, homogeneous, well crystal distributed, which made it more suitable for optical waveguide application.
Nanoporous g-Al2O3 samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al2O3. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al2O3 samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al2O3, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al2O3 for all samples. Also BET specific area values (253-280 m2/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.
Nanocrystalline TiO2 particles were successfully synthesized via sol-gel and sonochemical combination using titanium tetraisopropoxide as a precursor at lower temperature for a short time. The effect of the reaction parameters (hydrolysis media, acid media, and reaction temperatures) on the synthesis of TiO2 particles were investigated in the present study. Characterizations of synthesized samples were prepared by X-ray diffraction (XRD) analysis. It was shown that the reaction parameters played a significant role in the synthesis of TiO2 particles.
Nanofibers of PVA /nickel nitrate/silica/alumina izopropoxide/boric acid composite were prepared by using sol-gel processing and electrospinning technique. By high temperature calcinations of the above precursor fibers, nanofibers of NiO/Al2O3/B2O3/SiO2 composite with diameters about 500 nm could be successfully obtained. The fibers were characterized by XRD and SEM analyses.
Thin ZnO films are deposited on glass substrates via sol–gel method and dip-coating. The films are prepared from zinc acetate dehydrate as a starting reagent. After that the as-prepared ZnO sol is aged for different periods (0, 1, 3, 5, 10, 15 and 30 days). Nanocrystalline thin films are deposited from various sols. The effect ZnO sols aging time on the structural and photocatalytic properties of the films is studied. The films surface is studied by Scanning Electron Microscopy. The effect of the aging time of the starting solution is studied in the photocatalytic degradation of Reactive Black 5 (RB5) by UV-vis spectroscopy. The experiments are conducted upon UV-light illumination and in complete darkness. The variation of the absorption spectra shows the degradation of RB5 dissolved in water, as a result of the reaction, occurring on the surface of the films and promoted by UV irradiation. The initial concentrations of dye (5, 10 and 20 ppm) and the effect of the aging time are varied during the experiments. The results show, that the increasing aging time of starting solution with respect to ZnO generally promotes photocatalytic activity. The thin films obtained from ZnO sol, which is aged 30 days have best photocatalytic degradation of the dye (97,22%) in comparison with the freshly prepared ones (65,92%). The samples and photocatalytic experimental results are reproducible. Nevertheless, all films exhibit a substantial activity in both UV light and darkness, which is promising for the development of new ZnO photocatalysts by sol-gel method.
Composite material based on Fe3Si micro-particles and Mn-Zn nano-ferrite was prepared using powder metallurgy technology. The sol-gel followed by autocombustion process was used for synthesis of Mn0.8Zn0.2Fe2O4 ferrite. 3 wt.% of mechanically milled ferrite was mixed with Fe3Si powder alloy. Mixed micro-nano powder system was homogenized by the Resonant Acoustic Mixing using ResodynLabRAM Mixer. This non-invasive homogenization technique was used to preserve spherical morphology of Fe3Si powder particles. Uniaxial cold pressing in the closed die at pressure 600 MPa was applied to obtain a compact sample. Microwave sintering of green compact was realized at 800°C, 20 minutes, in air. Density of the powders and composite was measured by Hepycnometry. Impulse excitation method was used to measure elastic properties of sintered composite. Mechanical properties were evaluated by measurement of transverse rupture strength (TRS) and Vickers hardness (HV). Resistivity was measured by 4 point probe method. Ferrite phase distribution in volume of the composite was documented by metallographic analysis. It has been found that nano-ferrite particle distributed among micro- particles of Fe3Si powder alloy led to high relative density (~93%) and suitable mechanical properties (TRS >100 MPa, HV ~1GPa, E-modulus ~140 GPa) of the composite. High electric resistivity (R~6.7 ohm.cm) of prepared composite indicate their potential application as soft magnetic material at medium and high frequencies.
It is well known that in recent years magnetic materials have received increased attention due to their properties. For this reason a significant number of patents that were published during the last decade are oriented towards synthesis and study of such materials. The aim of this work is to create and study ferrite nanocrystalline materials with spinel structure, using sol-gel technology with participation of auto-combustion. This method is perspective in that it is a cheap and low-temperature technique that allows for the fine control on the product’s chemical composition.
In this research, waterglass based aerogel powder was prepared by sol–gel process and ambient pressure drying. Inspired by limited dust releasing, aerogel powder was introduced to the PET electrospinning solution in an attempt to create required bulk and surface structure for the nanofibers to improve their hydrophobic and insulation properties. The samples evaluation was carried out by measuring density, porosity, contact angle, heat transfer, FTIR, BET, and SEM. According to the results, porous silica aerogel powder was fabricated with mean pore diameter of 24 nm and contact angle of 145.9º. The results indicated the usefulness of the aerogel powder confined into nanofibers to control surface roughness for manipulating superhydrophobic nanowebs with water contact angle of 147º. It can be due to a multi-scale surface roughness which was created by nanowebs structure itself and nanofibers surface irregularity in presence of the aerogels while a layer of fluorocarbon created low surface energy. The wettability of a solid substrate is an important property that is controlled by both the chemical composition and geometry of the surface. Also, a decreasing trend in the heat transfer was observed from 22% for the nanofibers without any aerogel powder to 8% for the nanofibers with 4% aerogel powder. The development of thermal insulating materials has become increasingly more important than ever in view of the fossil energy depletion and global warming that call for more demanding energysaving practices.
The contact resistance between source/drain electrodes and semiconductor layer is an important parameter affecting electron transporting performance in the thin film transistor (TFT). In this work, we introduced a transparent and the solution prossable single-walled carbon nanotube (SWCNT)/Al-doped ZnO nano particle (AZO NP) bilayer electrodes showing low contact resistance with indium-oxide (In2O3) sol gel thin film. By inserting low work function AZO NPs into the interface between the SWCNTs and the In2O3 which has a high energy barrier, we could obtain an electrical Ohmic contact between them. Finally, with the SWCNT-AZO NP bilayer electrodes, we successfully fabricated a TFT showing a field effect mobility of 5.38 cm2/V·s at 250°C.
In the present study, we have synthesized Cr and Fe doped zinc oxide (ZnO) nanostructures (Zn1-δCraFebO; where δ = a + b = 20%, a = 5, 6, 8 & 10% and b = 15, 14, 12 & 10%) via sol-gel method at different doping concentrations. The synthesized samples were characterized for structural properties by X-ray diffractrometer and field emission scanning electron microscope and the optical properties were carried out through photoluminescence and UVvisible spectroscopy. The particle size calculated through field emission scanning electron microscope varies from 41 to 96 nm for the samples synthesized at different doping concentrations. The optical band gaps calculated through UV-visible spectroscopy are found to be decreasing from 3.27 to 3.02 eV as the doping concentration of Cr increases and Fe decreases.
Magnetic powder of Sr-ferrite was prepared by conventional and sol-gel auto-combustion methods. In conventional method, strontium carbonate and ferric oxide powders were mixed together and then mixture was calcined. In sol-gel auto-combustion method, a solution containing strontium nitrate, ferric nitrate and citric acid was heated until the combustion took place automatically; then, as-burnt powder was calcined. Thermal behavior, phase identification, morphology and magnetic properties of powders obtained by these two methods were compared by DTA, XRD, SEM and VSM techniques. According to the results of DTA analysis, formation temperature of Sr-ferrite obtained by conventional and solgel auto-combustion methods were 1300°C and 1000°C, respectively. XRD results confirmed the formation of pure Sr-ferrite at the mentioned temperatures. Plate and hexagonal-shape particles of Srferrite were observed using SEM. The Sr-ferrite powder obtained by sol-gel auto-combustion method had saturation magnetization of 66.03 emu/g and coercivity of 5731 Oe in comparison with values of 58.20 emu/g and 4378 Oe obtained by conventional method.
This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nanocrystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nanocomposites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900−1200 ◦C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nanocrystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ∼4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nanoparticles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nanocrystals were found to be just moderately modified in comparison to the bulk phases.
TiO2 thin films have been prepared by the sol-gel dipcoating technique in order to elaborate antireflective thin films for monocrystalline silicon (mono-Si). The titanium isopropoxyde was chosen as a precursor with hydrochloric acid as a catalyser for preparing a stable solution. The optical properties have been tailored with varying the solution concentration, the withdrawn speed, and the heat-treatment. We showed that using a TiO2 single layer with 64.5 nm in thickness, heat-treated at 450°C or 300°C reduces the mono-Si reflection at a level lower than 3% over the broadband spectral domains [669-834] nm and [786-1006] nm respectively. Those latter performances are similar to the ones obtained with double layers of low and high refractive index glasses respectively.
In this paper, strontium ferrite (SrO.6Fe2O3) was synthesized by the sol-gel auto-combustion process. The thermal behavior of powder obtained from self-propagating combustion of initial gel was evaluated by simultaneous differential thermal analysis (DTA) and thermo gravimetric (TG), from room temperature to 1200°C. The as-burnt powder was calcined at various temperatures from 700-900°C to achieve the single-phase Sr-ferrite. Phase composition, morphology and magnetic properties were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. Results showed that the single-phase and nano-sized hexagonal strontium ferrite particles were formed at calcination temperature of 800°C with crystallite size of 27 nm and coercivity of 6238 Oe.
Sol-gel method has been used to fabricate nanocomposite films on glass substrates composed halloysite clay mineral and nanocrystalline TiO2. The methodology for the synthesis involves a simple chemistry method utilized nonionic surfactant molecule as pore directing agent along with the acetic acid-based solgel route with the absence of water molecules. The thermal treatment of composite films at 450oC ensures elimination of organic material and lead to the formation of TiO2 nanoparticles onto the surface of the halloysite nanotubes. Microscopy techniques and porosimetry methods used in order to delineate the structural characteristics of the materials. The nanocomposite films produced have no cracks and active anatase crystal phase with small crystallite size were deposited on halloysite nanotubes. The photocatalytic properties for the new materials were examined for the decomposition of the Basic Blue 41 azo dye in solution. These, nanotechnology based composite films show high efficiency for dye’s discoloration in spite of different halloysite quantities and small amount of halloysite/TiO2 catalyst immobilized onto glass substrates. Moreover, we examined the modification of the halloysite/TiO2 films with silver particles in order to improve the photocatalytic properties of the films. Indeed, the presence of silver nanoparticles enhances the discoloration rate of the Basic Blue 41 compared to the efficiencies obtained for unmodified films.
In this paper, Zinc Oxide (ZnO) thin films are deposited on glass substrate by sol-gel method. The ZnO thin films with well defined orientation were acquired by spin coating of zinc acetate dehydrate monoethanolamine (MEA), de-ionized water and isopropanol alcohol. These films were pre-heated at 275°C for 10 min and then annealed at 350°C, 450°C and 550°C for 80 min. The effect of annealing temperature and different thickness on structure and surface morphology of the thin films were verified by Atomic Force Microscopy (AFM). It was found that there was a significant effect of annealing temperature on the structural parameters of the films such as roughness exponent, fractal dimension and interface width. Thin films also were characterizied by X-ray Diffractometery (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure and show the c-axis grain orientation. Increasing annealing temperature increased the crystallite size and the c-axis orientation of the film after 450°C. Also In this study, ZnO thin films in different thickness have been prepared by sol-gel method on the glass substrate at room temperature. The thicknesses of films are 100, 150 and 250 nm. Using fractal analysis, morphological characteristics of surface films thickness in amorphous state were investigated. The results show that with increasing thickness, surface roughness (RMS) and lateral correlation length (ξ) are decreased. Also, the roughness exponent (α) and growth exponent (β) were determined to be 0.74±0.02 and 0.11±0.02, respectively.
The powders of Ba(Ce1-xZrx)0.90Y0.1O3-δ (BCZY) with 0.2 ≤ x ≤ 0.6 have been prepared by a modified sol-gel method. Triethylenetetramine (TETA) was employed as chelating agent. Phase formation of calcined powders at 1100oC and sintered pellets at 1400oC of BCZY were examined by an X-ray diffractrometer (XRD). XRD results showed the calcined powder and sintered pellet formed a single perovskite phase over the entire range of x values. As the amount of zirconium substitution (x values) increase, the main peaks are shifted to the higher 2theta values which suggest a complete substitution of zirconium into cerium sites. All the obtained calcined powders and sintered pellets possess cubic structure (Pm-3m) at all x values.