• Bulletin of the Korean Chemical Society
• /
• v.34 no.2
• /
• pp.622-628
• /
• 2013

Nanocrystalline spinel lithium manganese oxide ($LiMn_2O_4$) powders with narrow-size-distribution, pure-phase particles, and high crystallinity with an average crystallite size of about 70 nm were synthesized at $600^{\circ}C$ for 6 h in air by freeze drying method. Spinel $LiMn_2O_4$ is also prepared by sol-gel using citric acid as a chelating agent. The influence of different parameters such as pH conditions, solvent, molar ratio of citric acid to total metal ions, calcination temperature, starting material on the structure, morphology and purity of this oxide was investigated. The results of sol-gel method show that pure $LiMn_2O_4$ with average crystallite size of about 130 nm can be produced from nitrate salts as starting materials at $800^{\circ}C$ for 6 h in air. The optimum pH and molar ratio of chelating agent to total metal ions are $4{\leq}pH{\leq}6$ and 1.0, respectively. A possible mechanism on the formation of the nanocrystallines synthesized by sol-gel was also discussed. At the end a comparison of the differences between two methods was made on the basis of x-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) tests.

• Advances in nano research
• /
• v.7 no.4
• /
• pp.233-240
• /
• 2019

The present research work reports in-vitro anti-cancer activity of biologically synthesized ZnO nanoparticles (ZnO NPs) against human carcinoma cells viz SCC-40, SK-MEL-2 and SCC-29B using Sulforhodamine-B (SRB) Assay. ZnO NPs were synthesized by a unique and novel biological route using Temperature-gradient phenomenon where the extract of combination of Catharanthus roseus (L.) G. Don (C. roseus), Azadirachta indica (A. indica), Ficus religiosa (F. religiosa) and NaOH solution were used as synthesis medium. The morphology of the ZnO NPs was characterized by Transmission Electron Microscopy (TEM). TEM images reveal that particle size of the samples reduces from 76 nm to 53 nm with the increase in reaction temperature and 68 nm to 38 nm with the increase in molar concentration of NaOH respectively. XRD study confirms the presence of elements and reduction in crystallite size with increase in reaction temperature and NaOH concentration. The diffraction peaks show broadening and a slight shift towards lower Bragg angle ($2{\theta}$) which represents the reduction in crystallite size as well as presence of uniform strain. The FTIR spectra of the extract show transmittance peak fingerprint of Zn-O bond and presence of bioactive molecules These NPs exhibit inhibition greater than 50% for SCC-40, SK-MEL-2 and SCC-29B cell lines and more than 50% cell kill for SCC-29B cells at concentrations < $80{\mu}g/ml$. Nanoparticles with smallest size have shown better anti-cancer activity and peculiar cell-selectivity. The combination of extracts of these plants with ZnO NPs can be used in targeted drug delivery as an effective anti-cancer agent, a potential application in cancer treatment.

• Korean Journal of Optics and Photonics
• /
• v.13 no.3
• /
• pp.197-203
• /
• 2002

The TiO$_2$ coating solutions were synthesized with different concentrations (T1-0.7N, T2-2.0N) of hydrochloric acid used as catalyst. and TiO$_2$ thin films were prepared by sol-gel dip coating. Their structural and optical properties were examined as a function of calcination temperature. XRD results showed that T1 thin films calcined at 400~80$0^{\circ}C$ had the anatase phase, while those calcined at 100$0^{\circ}C$ had the rutile phase. T2 thin films calcined at 40$0^{\circ}C$ and $600^{\circ}C$ had the anatase phase, with the rutile phase for calcination at 80$0^{\circ}C$. Crystallinity of T2 thin films was superior to that of T1 thin films. The crystallite size of TiO$_2$ thin films increased with increasing calcination temperature, and the crystallite size of anatase phase in T2 thin films was larger than that in T1 thin films, but the crystallite size of rutile phase in T2 thin films was smaller. The surface morphology of the films showed that the films were formed more densely in the rutile phase than in the anatase phase, this phenomenon appeared conspicuously in T2 thin films. The transmittance of the samples with thin films on quartz glass calcined at 100$0^{\circ}C$ was significantly reduced at wavelength range about 300-700 nm due to the increased absorption originating from the change of crystallite phase and composition of the films and the scattering effect originating from increasing crystallite size. The refractive index of TiO$_2$ thin films increased, and hence the film thickness as well as the porosity of TiO$_2$ thin films decreased with increasing calcination temperature. Furthermore, the refractive index of T2 thin films was higher than T1 thin films, and porosity of T2 films was lower.

• Environmental Engineering Research
• /
• v.16 no.2
• /
• pp.81-90
• /
• 2011

Different weight percentages of Ag, Pt, and Au doped nano $TiO_2$ were synthesized using the acetic acid hydrolyzed sol-gel method. The crystallite phase, surface morphology combined with elemental composition and light absorption properties of the doped nano $TiO_2$ were comprehensively examined using X-ray diffraction (XRD), $N_2$ sorption analysis, transmission electron microscopic (TEM), energy dispersive X-ray, and DRS UV-vis analysis. The doping of noble metals stabilized the anatase phase, without conversion to rutile phase. The formation of gold nano particles in Au doped nano $TiO_2$ was confirmed from the XRD patterns for gold. The specific surface area was found to be in the range 50 to 85 $m^2$/g. TEM images confirmed the formation a hexagonal plate like morphology of nano $TiO_2$. The photocatalytic activity of doped nano $TiO_2$ was evaluated using 4-chlorophenol as the model pollutant. Au doped (0.5 wt %) nano $TiO_2$ was found to exhibit higher photocatalytic activity than the other noble metal doped nano $TiO_2$, pure nano $TiO_2$ and commercial $TiO_2$ (Degussa P-25). This enhanced photocatalytic activity was due to the cathodic influence of gold in suppressing the electron-hole recombination during the reaction.

• Journal of the Korean Ceramic Society
• /
• v.53 no.5
• /
• pp.529-534
• /
• 2016

Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.

• Korean Journal of Materials Research
• /
• v.31 no.9
• /
• pp.481-487
• /
• 2021

ZnO particles are successfully synthesized at 150 ℃ for 30 min using zinc acetate as the Zn source and 1,4-butanediol as solvent using a relatively facile and convenient glycol process. The effect of ammonium hydroxide amounts on the growth behavior and the morphological evolution of ZnO particles are investigated. The prepared ZnO nanoparticle with hexagonal structure exhibits a quasi-spherical shape with an average crystallite size of approximately 30 nm. It is also demonstrated that the morphology of ZnO particles can be controlled by 1,4-butanediol with an additive of ammonium hydroxide. The morphologies of ZnO particles are changed sequentially from a quasi-spherical shape to a rod-like shape and a hexagonal rod shape with a truncated pyramidal tip, exhibiting preferential growth along the [001] direction with increasing ammonium hydroxide amounts. It is demonstrated that much higher OH^- amounts can produce a nano-tip shape grown along the [001] direction at the corners and center of the (001) top polar plane, and a flat hexagonal symmetry shape of the bottom polar plane on ZnO hexagonal prisms. The results indicate that the presence of NH⁴⁺ and OH^- ions in the solution greatly affects the growth behaviors of ZnO particles. A sharp near-band-edge (NBE) emission peak centered at 383 nm in the UV region and a weak broad peak in the visible region between 450 nm and 700 nm are shown in the PL spectra of the ZnO synthesized using the glycol process, regardless of adding ammonium hydroxide. Although the broad peak of the deep-level-emission (DLE) increases with the addition of ammonium hydroxide, it is suggested that the prominent NBE emission peaks indicate that ZnO nanoparticles with good crystallization are obtained under these conditions.

• Biomaterials and Biomechanics in Bioengineering
• /
• v.4 no.1
• /
• pp.21-32
• /
• 2019

Eggshell is a waste material after the usage of egg. In this work, biowaste chicken eggshells were used for preparing carbonated hydroxyapatite (HA) nanoparticles of high purity through aqueous precipitation method at room temperature. The eggshell-derived HA will be a cost-effective bioceramics for biomedical applications and an effective material-recycling technology. Additionally, mulberry leaf extract was used as a template to regulate the morphology, size and crystallinity of HA, and the effects of pH value were also examined. Characterization of the samples was performed by X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Scanning electron microscopy (SEM) was used to determine the size, shape and morphology of HA. The results indicate that only one phase of HA were synthesized in the both absence and presence of mulberry leaf extract at pH of 7 and above, while DCPD or DCPA/DCPD phase was observed at pH 4 condition. The crystallite sizes of the HA samples obviously decreased when adding mulberry leaf extract as a template, while they decreased gradually as the solution pH levels increased. With increasing pH level from 7 to 14, the rod-like HA nanoparticles gradually changed to spherical shape at pH 14. Note that, the obtained product is Mg and Sr containing A- and B-type carbonate HA at alkaline pH and it can be a potential material for biomedical applications.

• Mycobiology
• /
• v.36 no.2
• /
• pp.93-98
• /
• 2008

Two Schiff base ligands $L_1\;and\;L_2$ were obtained by the condensation of glycylglycine respectively with imidazole-2-carboxaldehyde and indole-3-carboxaldehyde and their complexes with Zn(II) were prepared and characterized by microanalytical, conductivity measurement, IR, UV-Vis., XRD and SEM. The molar conductance measurement indicates that the Zn(II) complexes are 1:1 electrolytes. The IR data demonstrate the tetradentate binding of $L_1$ and tridentate binding of $L_2$. The XRD data show that Zn(II) complexes with $L_1\;and\;L_2$ have the crystallite sizes of 53 and 61 nm respectively. The surface morphology of the complexes was studied using SEM. The in vitro biological screening effects of the investigated compounds were tested against the bacterial species Staphylococcus aureus, Escherichia coli, Klebsiella pneumaniae, Proteus vulgaris and Pseudomonas aeruginosa and fungal species Aspergillus niger, Rhizopus stolonifer, Aspergillus flavus, Rhizoctonia bataicola and Candida albicans by the disc diffusion method. A comparative study of inhibition values of the Schiff base ligands and their complexes indicates that the complexes exhibit higher antimicrobial activity than the free ligands. Zinc ions are proven to be essential for the growth-inhibitor effect. The extent of inhibition appeared to be strongly dependent on the initial cell density and on the growth medium.

• Journal of the Korean institute of surface engineering
• /
• v.50 no.3
• /
• pp.177-182
• /
• 2017

The properties of electroless Ni-B thin film on diamond powder with different parameters (temperature, pH, surfactant etc.) were studied. The surface morphology, structure and composition distribution of the Ni-B film were observed by field effect scanning electron microscope (FE-SEM), energy-dispersive spectrometer (EDS), X-ray diffraction (XRD) and Auger electron spectroscopy (AES). The growth rate of Ni-B film was increased with increase of bath temperature. The B content in Ni-B film was reduced with increase of bath pH. As a result the structure of Ni-B film was changed from amorphous to crystalline structure. The PVP in solution plays multi-functional roles as a dispersant and a stabilizer. The Ni-B film deposited with adding 0.1 mM-PVP was strongly introduced an amorphous structure with higher B content (25 at.%). Also the crystallite size of Ni-B film was reduced from 12.7 nm to 5.4 nm.

• Journal of the Korean Ceramic Society
• /
• v.30 no.4
• /
• pp.279-288
• /
• 1993

A study on calcination and reduction of AUC(ammonium uranyl carbonate, (NH4)4UO2(CO3)3) has been carried out by using TG-DTA in N2, air and H2 atmospheres, respectively. Phases of various intermediate obtained during thermal analysis of AUC in different atmospheres were confirmed by XRD. Powder characteristics of each intermediate were investigated by measuring particle size and specific surface area, and also observed by SEM. As a results, regardless of applied atmosphere AUC was calcined into amorphous UO3, which was converted to $\alpha$-U3O8 Via $\alpha$-UO3 in both H2 and N2 atmosphere, but directly into $\alpha$-UO3 in air atmosphere. Further reduction of U3O8 was only detectable in hydrogen atmosphere. During calcination and reduction, average particle size was reduced to less than 30% of original value without morphology change. Specific surface area was dramatically increased with release of NH3, CO2 and H2O from AUC powder and reached maximum value around 25$0^{\circ}C$, and then gradually decreased with the increase of temperature due to sintering effect of uranium oxides such as UO3 and U3O8. It was also found that the change of average crystallite size and pore size were closely related to the changes of specific surface area of uranium oxides.