Volume 31 (2013): Issue 2 (April 2013)

Despite the wide application of gadolinium as a contrast agent for magnetic resonance imaging (MRI), there is a serious lack of information on its toxicity. Gadolinium and gadolinium oxide (Gd-oxide) are used as contrast agents for magnetic resonance imaging (MRI). There are methods for reducing toxicity of these materials, such as core nanoparticles coating or conjugating. Therefore, for toxicity evaluation, we compared the viability of commercial contrast agents in MRI (Gd-DTPA) and three nanoparticles with the same core Gd2O3 and small particulate gadolinium oxide or SPGO (< 40 nm) but different coatings of diethyleneglycol (DEG) as Gd2O3-DEG and methoxy polyethylene glycol-silane (mPEG-silane: 550 and 2000 Dalton) as SPGO-mPEG-silane550 and SPGO-mPEG-silane2000, respectively, in the SK-MEL3 cell line, by light microscopy, MTT assay using 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide, and the LDH assay detecting lactate dehydrogenase activity. The viability values were not statistically different between the three nanoparticles and Gd-DTPA. The MTT and LDH assay results showed that Gd2O3-DEG nanoparticles were more toxic than Gd-DTPA and other nanoparticles. Also, SPGO-mPEG-silane2000 was more biocompatible than other nanoparticles. The obtained results did not show any significant increase in cytotoxicity of the nanoparticles and Gd-DTPA, neither dose-dependent nor time-dependent. Therefore, DEG and PEG, due to their considerable properties and irregular sizes (different molecular weights), were selected as the useful surface covering materials of nanomagnetic particles that could reveal noticeable relaxivity and biocompatibility characteristics.

Two-dimensional nano-crystals, nanosheets, are a new special type of nanomaterials recently discovered. They have attracted interest due to their unique potential applications especially in electronics. In this mini review, we present the current status of liquid exfoliation of layered crystals — an original new method of production of nanosheets. This “top down” synthesis is a low-temperature physico-chemical process already used to graphene production.

This study was aimed to explore the nanoparticle synthesizing properties of a silver resistant Bacillus sp. isolated from a marine water sample. The 16SrDNA sequence analysis of the isolate proved it as a Bacillus strain. Very interestingly, the isolate was found to have the ability to form intracellular silver nanoparticles at room temperature within 24 hours. This was confirmed by the UV-Vis absorption analysis which showed a peak at 430 nm corresponding to the plasmon absorbance of silver nanoparticles. Further characterization of the nanoparticles was carried out by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) analysis. The presence of silver nanoparticles with the size less than 100 nm was confirmed. These particles were found to be extremely stable as confirmed by the TEM analysis after three months of purification. So, the current study is the demonstration of an efficient synthesis of stable silver nanoparticles by a marine Bacillus strain.

ZnO nanorod arrays were grown on a flexible Kapton tape using microwave-assisted chemical bath deposition. High crystalline properties of the produced nanorods were proven by X-ray diffraction patterns and field emission scanning electron microscopy. Additionally, the photoluminescence spectrum showed higher UV peaks compared with visible peaks, which indicates that the ZnO nanorods had high quality and low number of defects. The metal-semiconductor-metal (MSM) configuration was used to fabricate UV and hydrogen gas detectors based on the ZnO nanorods grown on a flexible Kapton tape. Upon exposure to 395 nm UV light, the UV device exhibited fast response and decay times of 37 ms and 44 ms, respectively, at a bias voltage of 30 V. The relative sensitivities of the gas sensor made of the ZnO nanorod arrays, at hydrogen concentration of 2 %, at room temperature, 150 °C and 200 °C, are 0.42, 1.4 and 1.75 respectively.

Crystalline zirconium dioxide nanorods have been prepared by a simple hydrothermal process using zirconium hydroxide as the zirconium raw material. Zirconium dioxide nanorods are composed of monoclinic zirconium dioxide phase, which has been confirmed by the X-ray diffraction analysis. Electron microscopy observations show that the zirconium dioxide nanorods have a single crystal structure, with the rod diameter of less than 100 nm and length of 1–2 μm. Hydrothermal temperature and reaction time play essential roles in the formation and growth of the zirconium dioxide nanorods. Nucleation and crystal growth process are proposed to explain the formation and growth of the zirconium dioxide nanorods.

CuInS2 (CIS) is studied widely as a promising absorber material for high efficient and low cost thin film solar cells. CIS thin films are prepared on soda lime glass substrates using Successive Ionic Layer Adsorption and Reaction (SILAR) technique at different deposition temperatures (40 to 70 °C). The structural, compositional and optical properties are studied with x-ray diffractometer, energy dispersive x-ray analyzer and spectrophotometer. The influence of the deposition temperature on the properties of CIS thin films is discussed in this paper in detail.

(Bi1/2 Na1/2)0.94Ba0.06Ti1−x (Mg1/3Nb2/3)xO3 ceramic samples with x = 0.0, 0.01, 0.05, 0.15, 0.20 were synthesized by solid state method. Microstructure, dielectric properties, impedance and conductivity of the ceramics were studied. Phase formation was confirmed by X-ray diffraction. Co-doping of the ceramics with Mg and Nb at x = 0.01 raised the dielectric constant from 6510 to 8225 at the frequency of 1 KHz. Further increase in (Mg1/3Nb2/3)4+ concentration up to 0.15 increased the transition temperature from 275 °C to 339 °C and lowered the dielectric constant. The ac impedance measurements showed a linear response with frequency at lower temperature indicating insulating behavior and a single semicircular arc with spike at higher temperature.

The aim of this work was to prepare BiFeO3 by modified solid-state sintering and mechanical activation processes and to investigate the structure and hyperfine interactions of the material. X-ray diffraction and Mössbauer spectroscopy were applied as complementary methods. In the case of sintering, BiFeO3 phase was obtained from the mixture of precursors with 3 and 5 % excess of Bi2O3 during heating at 1023 K. Small amounts of impurities such as Bi2Fe4O9 and sillenite were recognized. In the case of mechanical activation, the milling of stoichiometric amounts of Bi2O3 and Fe2O3 followed by isothermal annealing at 973 K resulted in formation of the mixture of BiFeO3, Bi2Fe4O9, sillenite and hematite. After separate milling of individual Bi2O3 and Fe2O3 powders, mixing, further milling and thermal processing, the amount of desired BiFeO3 pure phase was significantly increased (from 70 to 90 %, as roughly estimated). From Mössbauer spectra, the hyperfine interaction parameters of the desired BiFeO3 compound, paramagnetic impurities of Bi2Fe4O9 and sillenite were determined. The main conclusion is that the lowest amount of impurities was obtained for BiFeO3 with 3 % excess of Bi2O3, which was sintered at 1023 K. However, in the case of mechanical activation, the pure phase formed at a temperature by 50 K lower as compared to solid-state sintering temperature. X-ray diffraction and Mössbauer spectroscopy revealed that for both sintered and mechanically activated BiFeO3 compounds, thermal treatment at elevated temperature led to a partial eliminating of the paramagnetic impurities.

Nanocrystalline multiferroic BiFeO3 ceramics was prepared by a novel solution combustion method (SCM). The X-ray diffraction (XRD) studies on structural properties of the synthesized ceramics reveal that the BiFeO3 ceramics has rhombhohedral perovskite structure with an average crystallite size of 15 nm. The ferroelectric P-E hysteresis loop measurement at room temperature shows unsaturated behavior with a partial reversal of polarization. Investigations on temperature dependence of dielectric constant in BiFeO3 demonstrate a clear dielectric anomaly at approximately around 380 °C, which corresponds to antiferromagnetic to paramagnetic phase transition (TN) and also evidences a possible coupling among the electric and magnetic dipoles of BiFeO3. A room temperature variation of dielectric constant “ɛ” and dielectric loss “tan δ” as a function of frequency in the range of 100 Hz — 1 MHz, confirms that both dielectric constant and loss are strong functions of frequency.

In this study, the growth of copper on porous diatom silica by electroless deposition method has been demonstrated for the first time. Raman peaks of copper (145, 213, and 640 cm−1) appeared in the copper-coated, Amphora sp. and Skeletonema sp. diatom samples, confirming the successful deposition of copper. Scanning electron microscopy (SEM) indicated the presence of copper on the diatom silica surface. The 3D intricate structure of diatom was still evident by optical and scanning electron microscopy analyses when the diatom samples were immersed in the copper bath for only 5 hours. Incubating the diatom samples in the copper bath for 24 h produced a dense coating on the diatom surface and covered the intricate 3D structure of the diatom silica. These results present possibilities of the fabrication of hierarchically organized copper with 3D diatom replica structures.

Electroluminescence of Y2O3:Eu and Y2O3:Sm films, as well as the films coactivated with Eu and Sm, is studied. The electroluminescence spectra are measured. The physical mechanism of electroluminescence is analyzed It is shown that the increase in the heat treatment temperature and the content of doping impurities of the films enhances the intensity of electroluminescence. Additional doping of Y2O3:EuF3 films by the SmF3 impurity, practically does not influence the emission spectrum.

In this work, the molten salt synthesis technique was applied to the synthesis of YAlO3 powder using LiCl, NaCl or KCl salt as the flux. YAlO3 powder was synthesized by reacting equimolar amounts of Y2O3 and Al2O3 powders in LiCl salt. The synthesis temperature for YAlO3 using LiCl salt was 1300 °C which is by about 500 °C lower than that in the conventional mixed-oxide method. The synthesized powders have been characterized using powder X-ray diffraction (XRD) analysis and field emission scanning electron microscopy (FE-SEM). The effect of the salt type on the formation of YAlO3 has also been investigated.

Encapsulation of chlorate in sodalite with aluminogermanate host framework has been obtained by one pot hydrothermal synthesis at 393 K. The crystal structure of Na8[AlGeO4]6(ClO3)2; sodalite was refined from X-ray powder data in the space group P$\bar 4$3n: a = 9.169 Å, where Al-O-Ge angle is 137.6°. The 27Al MAS NMR study confirmed alternate Ge and Al ordering of the sodalite framework, while 23Na gave insight into the structure and dynamics of the cage fillings. Infrared spectrum confirmed the encapsulation of chlorate as well as the framework formation of aluminogermanate sodalite. SEM study showed the retention of cubical morphology of the aluminogermanate sodalite. Thermogravimetric analysis provided information on the extent of chlorate entrapment, stability within the sodalite cages and decomposition properties.

In this study, some stabilized magnetite based ferrofluids were synthesized using Dextran as a stabilizing agent. In order to achieve optimum experimental conditions for synthesizing ferrofluids as MRI contrast agents, the Taguchi method was used. This approach was employed to design and minimize the number of required experiments. By using the Taguchi orthogonal (L16) array, four parameters including solution temperature and alkalinity, reaction temperature and stirring rate were selected at four predetermined levels for 16 experiments. Synthesizing processes established based on this set of experimental conditions were carried out and the obtained ferrofluids were characterized using PCS, VSM, TEM and FT-IR techniques. The obtained results were used and analyzed through the Qualitek-4 software and the proposed optimum experimental conditions were used for synthesizing the desired sample. Finally, this sample was used as a potential MRI contrast agent for imaging lymph nodes.

In this work, first principles calculations have been performed to study the doping and distribution of Si atoms in TiC lattice. The results confirm that Si atoms prefer to occupy Ti sites and their segregation on the TiC crystal surface may occur. But in the presence of carbon vacancies on the surface, Si atoms tend to be chemically adsorbed around the vacancies rather than occupy the carbon sites. It is also shown that the diffusion of Si may be very difficult in stoichiometric TiC, in particular the diffusion from bulk to surface. However, the carbon vacancies can considerably decrease the energy barrier and enhance the diffusion of Si atoms.

In this research work, we prepared γ-Fe2O3 nanoparticles by thermal-decomposition of Fe3O4. The Fe3O4 nanoparticles were synthesized via co-precipitation method at room temperature. This simple, soft and cheap method is suitable for preparation of iron oxide nanoparticles (γ-Fe2O3; Fe3O4). The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), vibrating sample magnetometer and differential scanning calorimeter (DSC). The XRD and FT-IR results indicated the formation of γ-Fe2O3 and Fe3O4 nanoparticles. The TEM images showed that the γ-Fe2O3 and Fe3O4 were spherical, and their size was 18 and 22 nm respectively. Magnetic properties have been measured by VSM at room temperature. Hysteresis loops showed that the γ-Fe2O3 and Fe3O4 nanoparticles were super-paramagnetic.

Here we report a successful preparation of nanostructured calcium silicate by wet chemical approach. The synthesized sample was characterized by various physico-chemical methods. Thermal stability was investigated using thermo-gravimetric and differential thermal analysis (TG-DTA). Structural characterization of the sample was carried out by the X-ray diffraction technique (XRD) which confirmed its single phase hexagonal structure. Transmission electron microscopy (TEM) was used to study the nanostructure of the ceramics while homogeneous grain distribution was revealed by scanning electron microscopy studies (SEM). The elemental analysis data obtained from energy dispersive X-ray spectroscopy (EDAX) were in close agreement with the starting composition used for the synthesis. Superhydrophilic nature of CaSiO3 was investigated at room temperature by sessile drop technique. Effect of porous nanosized CaSiO3 on early adhesion and proliferation of human bone marrow mesenchymal stem cells (BMMSCs) and cord blood mesenchymal stem (CBMSCs) cells was measured in vitro. MTT cytotoxicity test and cell adhesion test showed that the material had good biocompatibility and promoted cell viability and cell proliferation. It has been stated that the cell viability and proliferation are significantly affected by time and concentration of CaSiO3. These findings indicate that the CaSiO3 ceramics has good biocompatibility and that it is promising as a biomaterial.

Single-wall carbon nanotubes (SWNTs) as well as multi-wall carbon nanotubes (MWNTs) were characterized by Raman spectroscopy to observe the changes in their physical and structural properties on functionalization. When SWNTs or MWNTs are chemically treated, the defects are created. The analysis of radial breathing mode (RBM) showed that the diameter of the single wall carbon nanotubes changed after functionalization. In the carboxylated sample, the intensity of the disordered band (D-mode) increased more than in the pristine samples. The increase in the D-band intensity in SWNTs after functionalization can be attributed to carbon atoms excited from sp 2 to sp 3 hybridization. A higher intensity ratio in D-and G-mode (ID/IG) was observed after functionalization with carboxylic group (COOH). The intensity ratio ID/IG increased on acid treatment which was evident from the Raman spectra and their analysis. In case of MWNTs, the intensity of D band became equal to the intensity of G band, which was due to the huge number of defects that had been introduced in the sidewalls. Moreover, it was found in this study that the MWNTs can be much easier chemically functionalized than SWNTs under the same physical conditions.

Biological performance of bioceramics such as calcium phosphate has been proved to be improved by substitution of different ions like Mg, Sr and Si. In this study, different amounts of Zn ions in nitrate form were incorporated into β-tricalcium phosphate in which various molar ratios of Ca:Zn were achieved: 3:0, 2.8:0.2, 2.6:0.4, 2.4:0.6, and 2.2:0.8. The mixtures were heated at different temperatures ranging from 800–1100 °C. The phase composition, amount of each phase and lattice parameters of β-tricalcium phosphate were determined by means of X-ray diffractometry and coupled software. Also, solubility of the heated mixtures was investigated by determining the amount of Ca and Zn released into a simulated body fluid during 120 h. The results revealed that only limited amount of Zn ions could be incorporated into β-tricalcium phosphate lattice and ZnO phase was formed when high content of zinc nitrate was introduced in initial mixture. Both a and c lattice parameters of β-tricalcium phosphate were reduced by adding Zn. The release rate of calcium ions into the simulated body fluid was approximately constant during 120 h while for Zn minor release was observed.

Hybrid field-effect transistors (FETs) based on poly(3-hexylthiophene) (P3HT) containing CdSe quantum dots (QDs) were fabricated. The effect of the concentration of QDs on charge transport in the hybrid material was studied. The influence of the QDs capping ligand on charge transport parameters was investigated by replacing the conventional trioctylphosphine oxide (TOPO) surfactant with pyridine to provide closer contact between the organic and inorganic components. Electrical parameters of FETs with an active layer made of P3HT:CdSe QDs blend were determined, showing field-effect hole mobilities up to 1.1×10−4 cm2/Vs. Incorporation of TOPO covered CdSe QDs decreased the charge carrier mobility while the pyridine covered CdSe QDs did not alter this transport parameter significantly.