• Nuclear Engineering and Technology
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• v.50 no.3
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• pp.416-424
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• 2018

Microstructure of oxide formed on Zr-Nb-Sn tube sample was intensively examined by scanning transmission electron microscopy after exposure to simulated primary water chemistry conditions of various concentrations of Zn (0 or 30 ppb) and dissolved hydrogen ($H_2$) (30 or 50 cc/kg) for various durations without applying desirable heat flux. Microstructural analysis indicated that there was no noticeable change in the microstructure of the oxide corresponding to water chemistry changes within the test duration of 100 days (pretransition stage) and no significant difference in the overall thickness of the oxide layer. Equiaxed grains with nano-size pores along the grain boundaries and microcracks were dominant near the water/oxide interface, regardless of water chemistry conditions. As the metal/oxide interface was approached, the number of pores tended to decrease. However, there was no significant effect of $H_2$ concentration between 30 cc/kg and 50 cc/kg on the corrosion of the oxide after free immersion in water at $360^{\circ}C$. The adsorption of Zn on the cladding surface was observed by X-ray photoelectron spectroscopy and detected as ZnO on the outer oxide surface. From the perspective of $OH^-$ ion diffusion and porosity formation, the absence of noticeable effects was discussed further.

• Advances in materials Research
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• v.2 no.3
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• pp.141-153
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• 2013

Nanocrystalline Barium niobate ($BaNbO_3$) has been synthesized by a novel auto-igniting combustion technique. The X-Ray diffraction studies reveals that $BaNbO_3$ posses a cubic structure with lattice constant $a=4.071{\AA}$. Phase purity and structure of the nano powder are further examined using Fourier-Transform Infrared and Raman spectroscopy. The average particle size of the as prepared nano particles from the Transmission Electron Microscopy is 20 nm. The UV-Vis absorption spectra of the samples are recorded and the calculated average optical band gap is 3.74eV. The sample is sintered at an optimized temperature of $1425^{\circ}C$ for 2h and attained nearly 98% of the theoretical density. The morphology of the sintered pellet is studied with Scanning Electron Microscopy. The dielectric constant and loss factor of a well-sintered $BaNbO_3$ at 5MHz sample is found to be 32.92 and $8.09{\times}10^{-4}$ respectively, at room temperature. The temperature coefficient of dielectric constant was $-179pp/^{\circ}C$. The high dielectric constant, low loss and negative temperature coefficient of dielectric constant makes it a potential candidate for temperature sensitive dielectric applications.

• Nuclear Engineering and Technology
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• v.54 no.3
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• pp.1062-1070
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• 2022

In the present communication, pure and stable α-Bismuth Oxide (Bi₂O₃) nanoparticles (NPs) were synthesized by low temperature solution combustion method using urea as a fuel and calcined at 500℃. The synthesized sample was characterized by using powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray analysis (EDAX), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Visible absorption spectroscopy. The PXRD pattern confirms the formation of mono-clinic, stable and low temperature phase α-Bi₂O₃. The direct optical energy band gap was estimated by using Wood and Tauc's relation which was found to be 2.81 eV. The characterized sample was studied for X-ray/gamma ray shielding properties in the energy range 0.081-1.332 MeV using NaI (Tl) detector and multi channel analyzer (MCA). The measured shielding parameters agrees well with the theory, whereas, slight deviation up to 20% is observed below 356 keV. This deviation is mainly due to the influence of atomic size of the target medium. Furthermore an accurate theory is necessary to explain the interaction of X-ray/gamma ray with the NPs.The present work opens new window to use this facile, economical, efficient, low temperature method to synthesize nanomaterials for X-ray/gamma ray shielding purpose.

• Korean Journal of Crystallography
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• v.14 no.2
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• pp.79-83
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• 2003

The microstructure of bulk electrolytic MnO₂ (EMD) was studied using x-ray diffraction and transmission electron microscopy (TEM). The bulk sample showed a typical powder x-ray diffraction pattern of EMD materials. TEM study showed that the structure of EMD is present at two length scales;grains, ∼0.2 ㎛ in diameter, and ∼10 nm crystallites within the grain. The electron beam microdiffraction study revealed that each grain is an assemblage of multiphase with a common crystallographic orientation, and_that ∼50% of the crystallites are Ramsdellite, ∼30% are ε-MnO₂, and ∼15% are Pyrolusite. The ｛1120｝peak located at about 67° in powder XRD pattern as well as a high-resolution electron microscope (HREM) image of (0001) plane support the existence of ε-MnO₂ phase.

• Korean Journal of Materials Research
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• v.27 no.12
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• pp.705-709
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• 2017

The electronic and optical characteristics of molybdenum disulphide ($MoS_2$) film significantly vary with its thickness, and thus a rapid and accurate estimation of the number of $MoS_2$ layers is critical in practical applications as well as in basic researches. Various existing methods are currently available for the thickness measurement, but each has drawbacks. Transmission electron microscopy allows actual counting of the $MoS_2$ layers, but is very complicated and requires destructive processing of the sample to the point where it will no longer be useable after characterization. Atomic force microscopy, particularly when operated in the tapping mode, is likewise time-consuming and suffers from certain anomalies caused by an improperly chosen set point, that is, free amplitude in air for the cantilever. Raman spectroscopy is a quick characterization method for identifying one to a few layers, but the laser irradiation causes structural degradation of the $MoS_2$. Optical microscopy works only when $MoS_2$ is on a silicon substrate covered with $SiO_2$ of 100~300 nm thickness. The last two optical methods are commonly limited in resolution to the micrometer range due to the diffraction limits of light. We report here a method of measuring the distribution of the number of $MoS_2$ layers using a low voltage field emission electron microscope with acceleration voltages no greater than 1 kV. We found a linear relationship between the FESEM contrast and the number of $MoS_2$ layers. This method can be used to characterize $MoS_2$ samples at nanometer-level spatial resolution, which is below the limits of other methods.

• Korean Journal of Materials Research
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• v.23 no.2
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• pp.143-148
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• 2013

Well-distributed $SnO_2$-Sn-$Ag_3Sn$ nanoparticles embedded in carbon nanofibers were fabricated using a co-electrospinning method, which is set up with two coaxial capillaries. Their formation mechanisms were successfully demonstrated. The structural, morphological, and chemical compositional properties were investigated by field-emission scanning electron spectroscopy (FESEM), bright-field transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). In particular, to obtain well-distributed $SnO_2$ and Sn and $Ag_3Sn$ nanoparticles in carbon nanofibers, the relative molar ratios of the Ag precursor to the Sn precursor including 7 wt% polyacrylonitrile (PAN) were controlled at 0.1, 0.2, and 0.3. The FESEM, bright-field TEM, XRD, and XPS results show that the nanoparticles consisting of $SnO_2$-Sn-$Ag_3Sn$ phases were in the range of ~4 nm-6 nm for sample A, ~5 nm-15 nm for sample B, ~9 nm-22 nm for sample C. In particular, for sample A, the nanoparticles were uniformly grown in the carbon nanofibers. Furthermore, when the amount of the Ag precursor and the Sn precursor was increased, the inorganic nanofibers consisting of the $SnO_2$-Sn-$Ag_3Sn$ nanoparticles were formed due to the decreased amount of the carbon nanofibers. Thus, well-distributed nanoparticles embedded in the carbon nanofibers were successfully synthesized at the optimum molar ratio (0.1) of the Ag precursor to the Sn precursor after calcination of $800^{\circ}C$.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.630-630
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• 2013

Recently, atomically smooth hexagonal boron nitride(h-BN) known as a white graphene has drawn great attention since the discovery of graphene. h-BN is a III-V compound and has a honeycomb structure very similar to graphene with smaller lattice mismatch. Because of strong covalent sp2bonds like graphene, h-BN provides a high thermal conductivity and mechanical strength as well as chemical stability of h-BN superior to graphene. While graphene has a high electrical conductivity, h-BN has a highly dielectric property as an insulator with optical band gap up to 6eV. Similar to the graphene, h-BN can be applied to a variety of field, such as gate dielectric layers/substrate, ultraviolet emitter, transparent membrane, and protective coatings. However, up until recently, obtaining and controlling good quality monolayer h-BN layers have been too difficult and challenging. In this work, we investigate the controlled synthesis of h-BN layers according to the growth condition, time, temperature, and gas partial pressure. h-BN is obtained by using chemical vapor deposition on Cu foil with ammonia borane (BH3NH3) as a source for h-BN. Scanning Transmission Electron Microscopy (STEM, JEOL-JEM-ARM200F) is used for imaging and structural analysis of h-BN layer. Sample's surface morphology is characterized by Field emission scanning electron microscopy (SEM, JEOL JSM-7100F). h-BN is analyzed by Raman spectroscopy (HORIBA, ARAMIS) and its topographic variations by Atomic force microscopy (AFM, Park Systems XE-100).

• Applied Microscopy
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• v.39 no.3
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• pp.277-281
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• 2009

Practical difficulties for preparing a good crosssectional specimen of GaN-based materials for transmission electron microscopy have arisen due to large difference of mechanical properties between hard ceramic substrate and soft GaN-layered materials. Uneven polishing, sudden cracking, delamination, and selective sputtering during the conventional wedge polishing technique are often encountered as experimental hindrances. The preparation technique based on Strecker's method can be applied to overcome these difficulties, which eventually leads to mechanically stable TEM samples independent of the mechanical properties of materials. The basic idea is to use hard ceramic dummy filler for embedding the sample of interest into the dummy frame. In this study, we applied this technique into preparing cross-sectional TEM specimen of the GaN-based materials with mechanical instability and demonstrated usefulness of this hard dummy filler method in which the possible modifications of the sample of interest during the preparation must be avoidable. In addition, practical precautions during the preparation were discussed.

• Bulletin of the Korean Chemical Society
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• v.35 no.9
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• pp.2660-2664
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• 2014

A simple method of depositing titanium dioxide ($TiO_2$) nanoparticles onto graphene oxide (GO) as a catalytic support was devised for photocatalytic degradation of methylene blue (MB). Thiol groups were utilized as linkers to secure the $TiO_2$ nanoparticles. The resultant GO-supported $TiO_2$ (GO-$TiO_2$) sample was characterized by transmission electron microscopy (TEM), near-edge X-ray absorption fine structure (NEXAFS), and X-ray photoelectron spectroscopy (XPS) measurements, revealing that the anatase $TiO_2$ nanoparticles had effectively anchored to the GO surface. In the photodegradation of MB, GO-$TiO_2$ exhibited remarkably enhanced photocatalytic efficiency compared with thiolated GO and pure $TiO_2$ nanoparticles. Moreover, after five-cycle photodegradation experiment, no obvious deactivation was observed. The overall results showed that thiolated GO provides a good support substrate and, thereby, enhances the photodegradation effectiveness of the composite photocatalyst.

• Transactions on Electrical and Electronic Materials
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• v.14 no.6
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• pp.295-298
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• 2013

Nano-size manganese ferrite reinforced conductive polypyrrole composites reveal a core-shell structure by in situ polymerization, in the presence of dodecyl benzene sulfonic acid as the surfactant and dopant, and iron chloride as the oxidant. The structure and magnetic properties of manganese ferrite nano-fillers were measured, by using X-ray diffraction and vibrating sample magnetometer. The morphology, microstructure, and conductivity of the composite were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, and four-wire technique. The microwave-absorbing properties of composites reinforcement dispersed in resin coating with the coating thickness of 1.2 nm were investigated, by using vector network analyzers, in the frequency range of 8~12 GHz. A reflection loss of -8 dB was observed at 10.5 GHz.